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_7711892
_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_formula_moiety         'C23 H30 P W Zr, C24 B F20'
_chemical_formula_sum            'C47 H30 B F20 P W Zr'
_chemical_formula_weight         1291.56
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_update_record
;
2022-12-06 deposited with the CCDC.	2022-12-08 downloaded from the CCDC.
;
_cell_angle_alpha                98.483(3)
_cell_angle_beta                 107.679(3)
_cell_angle_gamma                115.933(3)
_cell_formula_units_Z            4
_cell_length_a                   16.6914(18)
_cell_length_b                   17.9195(19)
_cell_length_c                   18.449(2)
_cell_measurement_reflns_used    9763
_cell_measurement_temperature    123.(2)
_cell_measurement_theta_max      28.2876
_cell_measurement_theta_min      2.3803
_cell_volume                     4467.9(9)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_collection       'Bruker Instrument Service vV6.2.10'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 924)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123.(2)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker d8 Venture'
_diffrn_measurement_method       'omega- and phi-scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_type           Mo-Ka
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            63721
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.23
_diffrn_source                   'Incoatec ImuS3.0 microfocus sealed-tube'
_exptl_absorpt_coefficient_mu    2.961
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4656
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            'clear intense red-orange'
_exptl_crystal_density_diffrn    1.920
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2504
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.500
_exptl_crystal_size_min          0.280
_refine_diff_density_max         3.524
_refine_diff_density_min         -2.634
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1297
_refine_ls_number_reflns         20278
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0278
_refine_ls_R_factor_gt           0.0264
_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^)+(0.0167P)^2^+12.6408P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0619
_refine_ls_wR_factor_ref         0.0626
_reflns_number_gt                19435
_reflns_number_total             20278
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03833a3.cif
_cod_data_source_block           ZrCp2WCp2H2PMe3
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7711889--7711894.cif.

2024-10-08
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C94 H60 B2 F40 P2 W2 Zr2'
_cod_original_formula_weight         2583.12
_cod_original_formula_moiety         '2(C23 H30 P W Zr), 2(C24 B F20)'
_cod_original_formula_units_Z            2
_cod_original_cell_volume        4467.9(8)
_cod_database_code               7711892
_shelx_res_checksum              59950
_shelx_hkl_checksum              55305