Synthesis and Characterization of Organotriphosphonate-Functionalized TM-Containing Polyoxotungstates
Huo, Yu; Li, Dandan; Wan, Rong; Ma, Pengtao; Zhang, Dongdi; Niu, Jingyang; Wang, Jingping; RSC Adv.  (2015) –; doi:10.1039/C5RA20806H

data_7223385
_publ_section_title
;
 Synthesis and Characterization of Organotriphosphonate-Functionalized
 TM-Containing Polyoxotungstates
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA20806H
_journal_year                    2015
_chemical_formula_moiety
'0.5(C12 H24 As4 Co4 K8 N4 O230 P12 W56), 19(O)'
_chemical_formula_sum            'C6 H74 As2 Co2 K4 N2 O134 P6 W28'
_chemical_formula_weight         8076.05
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-11-21
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2015-11-22 deposited with the CCDC.
2015-11-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 122.1840(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.8801(12)
_cell_length_b                   27.6391(11)
_cell_length_c                   20.6261(8)
_cell_measurement_reflns_used    9163
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.12
_cell_measurement_theta_min      2.18
_cell_volume                     14416.8(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_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  0.0470
_diffrn_reflns_av_unetI/netI     0.0534
_diffrn_reflns_laue_measured_fraction_full 0.992
_diffrn_reflns_laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            37039
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.099
_diffrn_reflns_theta_max         25.099
_diffrn_reflns_theta_min         1.879
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    23.207
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.3681
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1437 before and 0.0489 after correction.
The Ratio of minimum to maximum transmission is 0.4936.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    3.714
_exptl_crystal_description       block
_exptl_crystal_F_000             14160
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_refine_diff_density_max         4.108
_refine_diff_density_min         -1.625
_refine_diff_density_rms         0.314
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     791
_refine_ls_number_reflns         12743
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0381
_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^)+(0.0568P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0969
_refine_ls_wR_factor_ref         0.1038
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9726
_reflns_number_total             12743
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra20806h1.cif
_cod_data_source_block           2
_cod_database_code               7223385
_shelx_estimated_absorpt_t_max   0.119
_shelx_estimated_absorpt_t_min   0.080
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Restrained distances
 O5W-O10W
 2.7 with sigma of 0.02
3. Rigid bond restraints
 N1, C3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 P2, C2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Co1, O36
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Co1, O37
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Co1, O51
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Co1, O52
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Others
 Fixed Sof: O7W(0.6) O8W(0.4) O9W(0.5) O10W(0.5) O11W(0.5) O12W(0.5) O13W(0.5)
 O14W(0.5) O15W(0.5) O16W(0.5) O17W(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B)
;
_shelx_res_checksum              33883
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'