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_7228093
_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         'Cd2 Cs3 Nb6 O46 P4, 10(O)'
_chemical_formula_sum            'Cd2 Cs3 H40 Nb6 O56 P4'
_chemical_formula_weight         2241.19
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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)
;
_audit_update_record
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2017-03-27 deposited with the CCDC.
2017-04-19 downloaded from the CCDC.
;
_cell_angle_alpha                72.1430(10)
_cell_angle_beta                 72.4400(10)
_cell_angle_gamma                72.8530(10)
_cell_formula_units_Z            1
_cell_length_a                   10.4234(4)
_cell_length_b                   10.9750(5)
_cell_length_c                   13.5568(6)
_cell_measurement_reflns_used    5584
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.46
_cell_volume                     1371.94(10)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0164
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7164
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.100
_diffrn_reflns_theta_max         25.100
_diffrn_reflns_theta_min         2.000
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.167
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5196
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0926 before and 0.0250 after correction.
The Ratio of minimum to maximum transmission is 0.6968.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.713
_exptl_crystal_description       block
_exptl_crystal_F_000             1055
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_refine_diff_density_max         2.750
_refine_diff_density_min         -2.806
_refine_diff_density_rms         0.220
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         4855
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0478
_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^)+(0.0681P)^2^+18.3491P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1264
_refine_ls_wR_factor_ref         0.1299
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4441
_reflns_number_total             4855
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce00603a2.cif
_cod_data_source_block           njy1
_cod_database_code               7228093
_shelx_estimated_absorpt_t_max   0.505
_shelx_estimated_absorpt_t_min   0.293
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(O9W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
2. Others
 Sof(Cs1')=1-FVAR(1)
 Sof(Cs1)=FVAR(1)
 Fixed Sof: Cs2(0.5) O9W(0.5) O10W(0.5) O11W(0.5) O12W(0.5)
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_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'