The firing of Josep Lluis Trapero, the highest-ranking officer of the Mossos d'Esquadra regional police, follows yesterday's dismissal of Catalonia's president, his deputy, all ministers, and the entire parliament.
Moving to quash what he termed an "escalation of disobedience", Prime Minister Mariano Rajoy called December 21 elections in the region under sweeping powers granted by the Senate in response to Catalan lawmakers voting to declare an independent republic.
The dismissal of Trapero, seen as an ally of his region's separatist leaders, was announced in today's official government gazette.
Instead, the ballot was disrupted, violently in some cases, by officers from Spain's national police and Guardia Civil paramilitary forces.
All eyes this weekend will be on whether Catalonia's separatist executive, led by Carles Puigdemont, will willingly step aside for caretaker envoys from Madrid.
Spain's Deputy Prime Minister Soraya Saenz de Santamaria is due to meet later with secretaries of state who will likely take charge of Catalonia's regional ministries.
Tens of thousands celebrated in Barcelona and other Catalan cities after yesterday's independence declaration, which analysts say the region has no legal power to execute.
The move to quash Catalan powers under Article 155 of the Spanish constitution is likely to anger many in a region of some 7.5 million people that enjoyed considerable autonomy, with control over education, healthcare and police.
It is the first time the central government has curtailed autonomy in the region since dictator Francisco Franco's repressive 1939-75 rule.
Independence supporters have warned they will resist the temporary measure, implemented under a constitutional article devised to rein in rebel regions.
"We won't cave in to Rajoy's authoritarianism nor to 155," the far-left CUP party, an ally of Puigdemont, tweeted.
Catalan leaders point to the "Yes" vote in the deeply- divisive October 1 referendum as a mandate for independence, even though less than half of voters took part.
Echoing widely-held fears, Federico Santi, Europe analyst at political risk consultancy Eurasia Group, warned the crisis could become violent, with "more serious clashes between national police and pro-independence activists."
Speaking after the parliament's proclamation, Puigdemont urged activists to "maintain the momentum" in a peaceful manner.
The Spanish government has received unwavering support from the United States and its allies in the European Union.
EU President Donald Tusk insisted Madrid "remains our only interlocutor" in Spain, but urged it to exercise restraint.
"I hope the Spanish government favours force of argument, not argument of force," he tweeted.
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