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_1517767
_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), C10 H10 O10 Zr, 2(C4 H8 O)
;
_chemical_formula_sum            'C54 H68 O32 Zr7'
_chemical_formula_weight         1867.62
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 99.532(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.1666(6)
_cell_length_b                   25.6460(12)
_cell_length_c                   11.1679(6)
_cell_measurement_reflns_used    9927
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      52.4
_cell_measurement_theta_min      2.4
_cell_volume                     3154.1(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      101(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  'Triumph graphite'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_sigmaI/netI    0.0277
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            39966
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         0.79
_exptl_absorpt_coefficient_mu    1.204
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6435
_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    1.967
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.554
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     860
_refine_ls_number_reflns         12418
_refine_ls_number_restraints     178
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0197
_refine_ls_R_factor_gt           0.0191
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0210P)^2^+0.3728P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0415
_refine_ls_wR_factor_ref         0.0417
_reflns_number_gt                12252
_reflns_number_total             12418
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-404-192-196-1.cif
_cod_data_source_block           lo_21
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1517767