Assembly of niobium-phosphate cluster and in-situ transition-metal-containing derivatives
Zhao, Shufang; Liang, Zhijie; Geng, Qiaohua; Ma, Pengtao; Zhang, Chao; Niu, Jingyang; Wang, Jingping; CrystEngComm  (2017) –; doi:10.1039/C7CE00603A

data_7228090
_publ_section_title
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 Assembly of niobium-phosphate cluster and in-situ
 transition-metal-containing derivatives
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE00603A
_journal_year                    2017
_chemical_formula_moiety         '0.5(Cs6 Nb12 Ni4 O100 P8)'
_chemical_formula_sum            'Cs3 H28 Nb6 Ni2 O50 P4'
_chemical_formula_weight         2025.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_primary     direct
_audit_creation_date             2017-03-25
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
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_audit_update_record
;
2017-03-27 deposited with the CCDC.
2017-04-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.3990(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.6885(7)
_cell_length_b                   20.2170(15)
_cell_length_c                   10.7300(7)
_cell_measurement_reflns_used    4116
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.08
_cell_measurement_theta_min      3.48
_cell_volume                     2173.2(3)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.1204
_diffrn_reflns_av_unetI/netI     0.0838
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            10922
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.099
_diffrn_reflns_theta_max         25.099
_diffrn_reflns_theta_min         2.033
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.130
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.3891
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1617 before and 0.0810 after correction.
The Ratio of minimum to maximum transmission is 0.5218.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'light green'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    3.096
_exptl_crystal_description       block
_exptl_crystal_F_000             1910
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         4.036
_refine_diff_density_min         -2.918
_refine_diff_density_rms         0.418
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         3840
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.1077
_refine_ls_R_factor_gt           0.0902
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1875P)^2^+24.9978P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2388
_refine_ls_wR_factor_ref         0.2651
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2991
_reflns_number_total             3840
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce00603a2.cif
_cod_data_source_block           njy1
_cod_database_code               7228090
_shelx_estimated_absorpt_t_max   0.513
_shelx_estimated_absorpt_t_min   0.360
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
O2 \\sim O1: within 1.5A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O5W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O15) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
2. Others
 Fixed Sof: Cs1(0.85) Cs2(0.15) Cs3(0.35) Cs4(0.15)
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_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'