Tweaking the bridge in metallocene Zr(IV)/W(IV) bimetallic hydrides.
Fernando, Selwin; Landrini, Martina; Macchioni, Alceo; Hughes, David L.; Budzelaar, Peter H. M.; Rocchigiani, Luca; Dalton transactions (Cambridge, England : 2003) 52 (2023) 394–408; doi:10.1039/d2dt03833a

data_7711891
_publ_section_title
;
 Tweaking the bridge in metallocene Zr(IV)/W(IV) bimetallic hydrides.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              394
_journal_page_last               408
_journal_paper_doi               10.1039/d2dt03833a
_journal_volume                  52
_journal_year                    2023
_chemical_absolute_configuration ad
_chemical_formula_moiety         'W Zr2 C30 H31, C24 B F20, W0.02 Zr0.04'
_chemical_formula_structural     'W(C5H4)2-H2-(ZrCp2)2H] [B(C6F5)4], 0.02(WZr2)'
_chemical_formula_sum            'C54 H31 B F20 W1.02 Zr2.04'
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_space_group_crystal_system      monoclinic
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_space_group_name_Hall           'P -2yc'
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_atom_sites_solution_hydrogens   mixed
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_atom_sites_solution_secondary   difmap
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_audit_update_record
;
2022-12-06 deposited with the CCDC.	2022-12-08 downloaded from the CCDC.
;
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_cell_length_b                   8.23727(11)
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'SHELXL-2018/3 (Sheldrick, 2015b) and WINGX (Farrugia, 2012)'
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_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'four-circle diffractometer'
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_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
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_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.988
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_diffrn_reflns_theta_max         28.999
_diffrn_reflns_theta_min         2.116
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
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_exptl_absorpt_correction_T_min  0.69489
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.035
_exptl_crystal_description       block
_exptl_crystal_F_000             1394
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.765
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details
;
 Flack x determined using 5885 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.0005(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     716
_refine_ls_number_reflns         12379
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0186
_refine_ls_R_factor_gt           0.0181
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0252P)^2^+0.8750P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0432
_refine_ls_wR_factor_ref         0.0434
_reflns_Friedel_coverage         0.974
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.976
_reflns_number_gt                12232
_reflns_number_total             12379
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03833a3.cif
_cod_data_source_block           lucar21-2021ncs0040r1z
_cod_depositor_comments
'Adding full bibliography for 7711889--7711894.cif.'
_cod_original_sg_symbol_H-M      'P c'
_cod_database_code               7711891
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              12265
_shelx_hkl_checksum              17257