Synthesis and Crystal Structure of [Cp3Zr3(u2-O2CH)3(u2-OH)3(u3-O)]2 [CpZr(O2CH)5] and [Cp3Zr3(u2-O2CH)3(u2-OH)3(u3-O)] [B(C6F5)4]
Lars Orzechowski; Joachim Roll; Inorganica Chimica Acta 404 (2013) 192–196; doi:

data_1517768
_publ_section_title
;
 Synthesis and Crystal Structure of [Cp3Zr3(u2-O2CH)3(u2-OH)3(u3-O)]2
 [CpZr(O2CH)5] and [Cp3Zr3(u2-O2CH)3(u2-OH)3(u3-O)] [B(C6F5)4]
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              192
_journal_page_last               196
_journal_volume                  404
_journal_year                    2013
_chemical_formula_moiety
;
 2[C18 H21 O10 Zr3], 2[C24 F20 B], 7[C4 H10 O], 2[C H Cl2]
;
_chemical_formula_sum            'C57 H58 B Cl2 F20 O13.5 Zr3'
_chemical_formula_weight         1694.42
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                96.136(2)
_cell_angle_beta                 109.816(2)
_cell_angle_gamma                118.5560(10)
_cell_formula_units_Z            2
_cell_length_a                   15.2956(7)
_cell_length_b                   15.6974(7)
_cell_length_c                   17.2726(13)
_cell_measurement_reflns_used    9049
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.35
_cell_volume                     3240.4(3)
_computing_cell_refinement       'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_data_collection       'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_data_reduction        'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_molecular_graphics    'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'
_computing_publication_material  'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'
_computing_structure_refinement  'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'
_computing_structure_solution    'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type
; 
 Bruker D8 KAPPA series II with APEX II area detector system
;
_diffrn_measurement_method
;
 Data collection strategy APEX 2/COSMO
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_sigmaI/netI    0.0172
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            93255
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.33
_exptl_absorpt_coefficient_mu    0.670
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.66
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 BRUKER AXS SMART APEX 2 Vers. 3.0-2009
 R.H. Blessing, Acta Cryst. (1995) A51 33-38 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.733
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.948
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     905
_refine_ls_number_reflns         15703
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0282
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0352P)^2^+3.1941P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0714
_refine_ls_wR_factor_ref         0.0748
_reflns_number_gt                13783
_reflns_number_total             15703
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-404-192-196-2.cif
_cod_data_source_block           lars_zr0m
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C57 H58 Cl2 B F20 O13.50 Zr3'
_cod_database_code               1517768