Immobilization of carbonyl rhenium tripods on the surface of a trinickel-substituted Dawson-type polyoxotungstate.
Jia, Jiage; Ma, Pengtao; Zhang, Panpan; Zhang, Dongdi; Zhang, Chao; Niu, Jingyang; Wang, Jingping; Dalton transactions (Cambridge, England : 2003) 47 (2018) 6288–6292; doi:10.1039/c8dt00138c

data_7045967
_publ_section_title
;
 Immobilization of carbonyl rhenium tripods on the surface of a
 trinickel-substituted Dawson-type polyoxotungstate.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6288
_journal_page_last               6292
_journal_paper_doi               10.1039/c8dt00138c
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C9 Ni3 O71 P2 Re3 W15, 20(O)'
_chemical_formula_sum            'C9 H46 Ni3 O91 P2 Re3 W15'
_chemical_formula_weight         5164.88
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_primary     direct
_audit_creation_date             2017-02-25
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2017-08-07 deposited with the CCDC.
2018-04-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.1100(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.5956(7)
_cell_length_b                   22.3215(11)
_cell_length_c                   14.8504(7)
_cell_measurement_reflns_used    6125
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.18
_cell_volume                     4837.3(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL-2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_av_unetI/netI     0.0549
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            25112
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.099
_diffrn_reflns_theta_max         25.099
_diffrn_reflns_theta_min         1.825
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    22.199
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.2740
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1608 before and 0.0521 after correction.
The Ratio of minimum to maximum transmission is 0.3674.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    3.546
_exptl_crystal_description       block
_exptl_crystal_F_000             4554
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         2.938
_refine_diff_density_min         -1.567
_refine_diff_density_rms         0.333
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         8806
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0406
_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^)+(0.0456P)^2^+79.4605P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0994
_refine_ls_wR_factor_ref         0.1100
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6786
_reflns_number_total             8806
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00138c2.cif
_cod_data_source_block           njy1
_cod_depositor_comments          'Adding full bibliography for 7045967.cif.'
_cod_database_code               7045967
_shelx_estimated_absorpt_t_max   0.160
_shelx_estimated_absorpt_t_min   0.046
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(P2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
2. Others
 Fixed Sof: O1W(0.5) O1BW(0.5)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'