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_4347495
_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
'C20 H40 Na O5, C102 H152 Na2 O10 P3 Zr2, 2.5(C4 H8 O)'
_chemical_formula_sum            'C132 H212 Na3 O17.5 P3 Zr2'
_chemical_formula_weight         2423.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 94.695(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.381(5)
_cell_length_b                   14.740(3)
_cell_length_c                   40.457(9)
_cell_measurement_reflns_used    19667
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.4468
_cell_measurement_theta_min      3.0464
_cell_volume                     13896(5)
_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 0.997
_diffrn_measured_fraction_theta_max 0.994
_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  0.0735
_diffrn_reflns_av_unetI/netI     0.1334
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            151258
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.455
_diffrn_reflns_theta_min         3.031
_diffrn_source                   'Rotationg Anode'
_exptl_absorpt_coefficient_mu    0.251
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9105
_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            Yellow
_exptl_crystal_density_diffrn    1.158
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             5208
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.963
_refine_diff_density_min         -0.612
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details
;
 Flack x determined using 11798 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.010(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3469
_refine_ls_number_reflns         62025
_refine_ls_number_restraints     8898
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.1216
_refine_ls_R_factor_gt           0.0918
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0947P)^2^+11.8151P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2030
_refine_ls_wR_factor_ref         0.2321
_reflns_Friedel_coverage         0.963
_reflns_Friedel_fraction_full    0.974
_reflns_Friedel_fraction_max     0.958
_reflns_number_gt                45323
_reflns_number_total             62025
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00233_si_001.cif
_cod_data_source_block           (O3C)Zr-CycloP3-Complex4
_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 

2024-02-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C264 H424 Na6 O35 P6 Zr4'
_cod_original_formula_weight         4846.65
_cod_original_formula_moiety
'2(C20 H40 Na O5), 2(C102 H152 Na2 O10 P3 Zr2), 5(C4 H8 O)'
_cod_original_formula_units_Z            2
_cod_original_sg_symbol_H-M      'P c'
_cod_database_code               4347495
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.951
_shelx_estimated_absorpt_t_max   0.970
_shelx_res_checksum              62881
_shelx_hkl_checksum              79651
_shelx_fab_checksum              41383