A series of organic‒inorganic hybrid materials consisting of flexible organic amine modified polyoxomolybdates: synthesis, structures and properties
Gong, Chunhua; Zeng, Xianghua; Zhu, Chengfeng; Shu, Jiahui; Xiao, Pingxiu; Xu, Hao; Liu, Lichun; Zhang, Junyong; Zeng, Qingdao; Xie, Jingli; RSC Advances 6 (2016) 106248–; doi:10.1039/C6RA21603J

data_7236261
_publ_section_title
;
 A series of organic--inorganic hybrid materials consisting of flexible
 organic amine modified polyoxomolybdates: synthesis, structures and
 properties
;
_journal_issue                   108
_journal_name_full               'RSC Advances'
_journal_page_first              106248
_journal_paper_doi               10.1039/C6RA21603J
_journal_volume                  6
_journal_year                    2016
_chemical_formula_moiety         'C36 H60 Mo5 N8 O23 P2 Zn2, 11(O)'
_chemical_formula_sum            'C36 H60 Mo5 N8 O34 P2 Zn2'
_chemical_formula_weight         1821.30
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-10-31
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2016.10.10 svn.r3347 for OlexSys, GUI svn.r5252)
;
_audit_update_record
;
2016-10-31 deposited with the CCDC.
2016-11-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.164(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8566(5)
_cell_length_b                   19.7359(8)
_cell_length_c                   26.2178(10)
_cell_measurement_reflns_used    7258
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.7950
_cell_measurement_theta_min      3.1610
_cell_volume                     6038.7(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0802
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -79.00  -36.50   0.8500   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.2084  132.0000 -141.0000 50

  2 omega  -14.00   25.10   0.8500   50.0000
omega____ theta____ kappa____ phi______ frames
    -       18.4428  -57.0000    0.0000 46

  3 omega  -48.00   59.10   0.8500   50.0000
omega____ theta____ kappa____ phi______ frames
    -       18.4428  -19.0000  150.0000 126

  4 omega   31.00   90.50   0.8500   50.0000
omega____ theta____ kappa____ phi______ frames
    -       18.4428   19.0000  -30.0000 70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0098296000
_diffrn_orient_matrix_UB_12      0.0023614000
_diffrn_orient_matrix_UB_13      0.0274079000
_diffrn_orient_matrix_UB_21      -0.0114276000
_diffrn_orient_matrix_UB_22      -0.0351332000
_diffrn_orient_matrix_UB_23      0.0016853000
_diffrn_orient_matrix_UB_31      0.0589186000
_diffrn_orient_matrix_UB_32      -0.0072078000
_diffrn_orient_matrix_UB_33      0.0007886000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_unetI/netI     0.0644
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            24542
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.874
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.938
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56315
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.003
_exptl_crystal_description       block
_exptl_crystal_F_000             3616
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.723
_refine_diff_density_min         -0.837
_refine_diff_density_rms         0.188
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     784
_refine_ls_number_reflns         10612
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0942
_refine_ls_R_factor_gt           0.0731
_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^)+(0.0364P)^2^+125.6111P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1708
_refine_ls_wR_factor_ref         0.1789
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8382
_reflns_number_total             10612
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra21603j2.cif
_cod_data_source_block           1
_cod_database_code               7236261
_chemical_oxdiff_formula         'Zn1 C18 N4 H18 P1 Mo7 O23'
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C12(H12A,H12B), C18(H18A,H18B), C24(H24A,H24B), C30(H30A,H30B),
 C36(H36A,H36B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C13(H13),
 C14(H14), C15(H15), C16(H16), C19(H19), C20(H20), C21(H21), C22(H22), C25(H25),
  C26(H26), C27(H27), C28(H28), C31(H31), C32(H32), C33(H33), C34(H34)
;
_shelx_res_checksum              71139
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 1450769351.08
_olex2_submission_special_instructions 'No special instructions were received'