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_7711890
_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         'C27 H30 N W Zr, B C24 F20'
_chemical_formula_sum            'C51 H30 B F20 N W Zr'
_chemical_formula_weight         1322.64
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2022-09-16
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-10-12 deposited with the CCDC.	2022-12-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.6400(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.7488(6)
_cell_length_b                   17.4771(6)
_cell_length_c                   18.3105(7)
_cell_measurement_reflns_used    9012
_cell_measurement_temperature    120.(2)
_cell_measurement_theta_max      28.2749
_cell_measurement_theta_min      2.5980
_cell_volume                     4522.2(3)
_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    'Olex2 1.5 (Dolomanov et al., 2009)'
_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      120.(2)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0192
_diffrn_reflns_av_unetI/netI     0.0146
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            56472
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.40
_diffrn_source                   'Incoatec ImuS3.0 microfocus sealed-tube'
_exptl_absorpt_coefficient_mu    2.895
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5804
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.943
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2568
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.223
_refine_diff_density_min         -0.866
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     684
_refine_ls_number_reflns         11162
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0197
_refine_ls_R_factor_gt           0.0191
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0217P)^2^+5.2833P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0490
_refine_ls_wR_factor_ref         0.0494
_reflns_number_gt                10895
_reflns_number_total             11162
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03833a3.cif
_cod_data_source_block           Cp2Zr35LutidineWCp2
_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.
;
_cod_database_code               7711890
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10),
 C16(H16), C12(H12), C13(H13), C14(H14), C15(H15), C18(H18), C19(H19), C11(H11),
  C17(H17), C20(H20)
1.b Aromatic/amide H refined with riding coordinates:
 C21(H21), C25(H25), C23(H23)
1.c Idealised Me refined as rotating group:
 C26(H02A,H02B,H02C), C27(H01E,H01G,H01I)
;
_shelx_res_checksum              71282
_shelx_hkl_checksum              13687
_olex2_submission_special_instructions 'No special instructions were received'