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_7223386
_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 H16 As4 K8 Mn4 N4 O232 P12 W56), 18(O)'
_chemical_formula_sum            'C6 H74 As2 K4 Mn2 N2 O134 P6 W28'
_chemical_formula_weight         8068.06
_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                 121.555(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.848(4)
_cell_length_b                   27.794(4)
_cell_length_c                   20.700(3)
_cell_measurement_reflns_used    4537
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.16
_cell_measurement_theta_min      2.48
_cell_volume                     14633(4)
_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 0.994
_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  0.1079
_diffrn_reflns_av_unetI/netI     0.1297
_diffrn_reflns_laue_measured_fraction_full 0.994
_diffrn_reflns_laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            37013
_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         1.866
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    22.809
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.2102
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1654 before and 0.0652 after correction.
The Ratio of minimum to maximum transmission is 0.2819.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.657
_exptl_crystal_description       block
_exptl_crystal_F_000             14152
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         5.201
_refine_diff_density_min         -2.377
_refine_diff_density_rms         0.570
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.956
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     785
_refine_ls_number_reflns         12968
_refine_ls_number_restraints     79
_refine_ls_restrained_S_all      0.955
_refine_ls_R_factor_all          0.1457
_refine_ls_R_factor_gt           0.0691
_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^)+(0.0937P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1578
_refine_ls_wR_factor_ref         0.1847
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7201
_reflns_number_total             12968
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra20806h1.cif
_cod_data_source_block           3
_cod_original_cell_volume        14634(4)
_cod_database_code               7223386
_shelx_estimated_absorpt_t_max   0.131
_shelx_estimated_absorpt_t_min   0.031
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Restrained distances
 O4W-O9W
 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
 Mn1, O36
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Mn1, O37
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Mn1, O51
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Mn1, O52
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(Mn1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C3) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O35) \\sim
Ueq, Uanis(O11) \\sim Ueq, Uanis(O21) \\sim Ueq, Uanis(O39) \\sim Ueq,
Uanis(O47) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(O22) \\sim Ueq, Uanis(O52)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: O7W(0.6) O8W(0.4) O10W(0.5) O11W(0.5) O12W(0.5) O14W(0.5)
 O15W(0.5) O16W(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B)
;
_shelx_res_checksum              41043
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'