Construction of a new binding manner in carboxylic acid-functionalized phosphomolybdates.
Wang, Jin; Shi, Wenjie; Li, Shujie; Mao, Qiyun; Ma, Pengtao; Niu, Jingyang; Wang, Jingping; Dalton transactions (Cambridge, England : 2003) 47 (2018) 7949–7955; doi:10.1039/c8dt01540f

data_7046330
_publ_section_title
;
 Construction of a new binding manner in carboxylic acid-functionalized
 phosphomolybdates.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7949
_journal_page_last               7955
_journal_paper_doi               10.1039/c8dt01540f
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C28 H12 Cs3.5 Mo18 N4 O90.5 P3, 11.5(O)'
_chemical_formula_sum            'C28 H54 Cs3.5 Mo18 N4 O102 P3'
_chemical_formula_weight         4363.76
_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_hydrogens   geom
_audit_creation_date             2015-11-11
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2018-03-30 deposited with the CCDC.
2018-05-14 downloaded from the CCDC.
;
_cell_angle_alpha                96.4300(10)
_cell_angle_beta                 94.7450(10)
_cell_angle_gamma                96.2270(10)
_cell_formula_units_Z            2
_cell_length_a                   12.2276(10)
_cell_length_b                   17.7227(14)
_cell_length_c                   33.640(3)
_cell_measurement_reflns_used    9939
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.62
_cell_measurement_theta_min      2.27
_cell_volume                     7168.1(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 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0251
_diffrn_reflns_av_unetI/netI     0.0520
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            36984
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.100
_diffrn_reflns_theta_max         25.100
_diffrn_reflns_theta_min         1.790
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.523
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.3908
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1002 before and 0.0379 after correction.
The Ratio of minimum to maximum transmission is 0.5241.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.022
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4119
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.45
_refine_diff_density_max         3.635
_refine_diff_density_min         -3.258
_refine_diff_density_rms         0.244
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     769
_refine_ls_number_reflns         25255
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0943
_refine_ls_R_factor_gt           0.0754
_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^)+(0.1242P)^2^+106.2531P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2065
_refine_ls_wR_factor_ref         0.2268
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19673
_reflns_number_total             25255
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01540f2.cif
_cod_data_source_block           njy1
_cod_depositor_comments
'Adding full bibliography for 7046330--7046333.cif.'
_cod_original_cell_volume        7168.0(10)
_cod_original_formula_sum        'C28 H54 Cs3.50 Mo18 N4 O102 P3'
_cod_database_code               7046330
_shelx_estimated_absorpt_t_max   0.396
_shelx_estimated_absorpt_t_min   0.365
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Fixed Sof: Cs2(0.5) Cs3(0.5) Cs4(0.5) Cs5(0.5) Cs6(0.5) Cs7(0.25) Cs8(0.25)
 O21W(0.5) O22W(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C10(H10), C11(H11), C12(H12), C17(H17), C18(H18),
 C19(H19), C24(H24), C25(H25), C26(H26)
;
_shelx_res_checksum              70841
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'