Zirconium Hydride Complex Supported by a Tetradentate Carbon-Centered Tripodal Tris(aryloxide) Ligand: Synthesis, Structure, and Reactivity.
Nakanishi, Yusuke; Ishida, Yutaka; Kawaguchi, Hiroyuki; Inorganic chemistry 55 (2016) 3967–3973; doi:10.1021/acs.inorgchem.6b00233

data_4347496
_publ_section_title
;
 Zirconium Hydride Complex Supported by a Tetradentate Carbon-Centered
 Tripodal Tris(aryloxide) Ligand: Synthesis, Structure, and Reactivity.
;
_journal_issue                   8
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3967
_journal_page_last               3973
_journal_paper_doi               10.1021/acs.inorgchem.6b00233
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C165 H252 N9 Na3 O18 Zr3 4(C5 H12)'
_chemical_formula_sum            'C185 H300 N9 Na3 O18 Zr3'
_chemical_formula_weight         3280.95
_space_group_crystal_system      cubic
_space_group_IT_number           205
_space_group_name_Hall           '-P 2ac 2ab 3'
_space_group_name_H-M_alt        'P a -3'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.4443(9)
_cell_length_b                   34.4443(9)
_cell_length_c                   34.4443(9)
_cell_measurement_reflns_used    38388
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.8
_cell_volume                     40865.1(18)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2009)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2009)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2009)'
_computing_molecular_graphics
'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_publication_material
'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku Saturn724+ CCD'
_diffrn_measurement_method       dtproprofit.ref
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1648
_diffrn_reflns_av_unetI/netI     0.0616
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            334006
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.456
_diffrn_reflns_theta_min         3.647
_diffrn_source                   'Rotationg Anode'
_exptl_absorpt_coefficient_mu    0.212
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.854
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Jacobson, R. (1998). REQAB. Private communication to the 
Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.067
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Chunk
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_exptl_crystal_size_mid          0.150
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_refine_diff_density_min         -0.554
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
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_refine_ls_number_restraints     822
_refine_ls_restrained_S_all      1.315
_refine_ls_R_factor_all          0.1308
_refine_ls_R_factor_gt           0.0994
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2933
_refine_ls_wR_factor_ref         0.3210
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10891
_reflns_number_total             15552
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00233_si_001.cif
_cod_data_source_block           (O3C)ZrN3-Complex5
_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/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        40865(3)
_cod_database_code               4347496
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.957
_shelx_estimated_absorpt_t_max   0.971
_shelx_res_checksum              51190
_shelx_hkl_checksum              74228
_shelx_fab_checksum              90508