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_7236266
_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
'2(C18 H24 Cr Cu Mo6 N4 O24), C36 H43 Cr Cu2 Mo6 N8 O24, 4(H2 O)'
_chemical_formula_sum            'C72 H99 Cr3 Cu4 Mo18 N16 O76'
_chemical_formula_weight         4541.75
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_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                99.314(3)
_cell_angle_beta                 116.519(4)
_cell_angle_gamma                91.546(3)
_cell_formula_units_Z            1
_cell_length_a                   14.4947(6)
_cell_length_b                   15.7549(4)
_cell_length_c                   15.8183(6)
_cell_measurement_reflns_used    8946
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.9390
_cell_measurement_theta_min      3.1090
_cell_volume                     3169.4(2)
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -22.00   23.05   0.8500   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.0522  -99.0000  -60.0000 53

  2 omega  -21.00   22.35   0.8500   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.0522  -99.0000   30.0000 51

  3 omega   -5.00   89.35   0.8500   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.2865   38.0000  -60.0000 111

  4 omega   55.00   80.50   0.8500   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.2865 -178.0000 -150.0000 30

  5 omega   37.00   93.10   0.8500   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.2865  178.0000  150.0000 66

  6 omega   19.00   52.15   0.8500   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.2865  -99.0000 -180.0000 39

  7 omega  -41.00   83.10   0.8500   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.2865    0.0000 -120.0000 146
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0144152000
_diffrn_orient_matrix_UB_12      -0.0041179000
_diffrn_orient_matrix_UB_13      0.0366282000
_diffrn_orient_matrix_UB_21      -0.0529827000
_diffrn_orient_matrix_UB_22      -0.0009899000
_diffrn_orient_matrix_UB_23      -0.0333283000
_diffrn_orient_matrix_UB_31      -0.0037667000
_diffrn_orient_matrix_UB_32      -0.0457176000
_diffrn_orient_matrix_UB_33      -0.0125521000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0227
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23137
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.700
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.718
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96787
_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            yellow
_exptl_crystal_density_diffrn    2.380
_exptl_crystal_description       block
_exptl_crystal_F_000             2195
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.757
_refine_diff_density_min         -0.557
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     868
_refine_ls_number_reflns         11152
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0280
_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^)+(0.0283P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0610
_refine_ls_wR_factor_ref         0.0651
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9230
_reflns_number_total             11152
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra21603j2.cif
_cod_data_source_block           7
_cod_database_code               7236266
_chemical_oxdiff_formula         'C21 H20 Mo4 N4 O13 Cu1'
_reflns_odcompleteness_completeness 99.88
_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
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Others
 Fixed Sof: H25(0.5) H28(0.5) H19(0.5) O2W(0.5) H2WA(0.5) H2WB(0.5) O3W(0.5)
 H3WA(0.5) H3WB(0.5)
3.a Riding coordinates:
 O14(H14), O15(H15), O22(H22), O25(H25), O26(H26), O28(H28), O30(H30),
 O19(H19), O20(H20), O27(H27), O36(H36), O1W(H1WA,H1WB), O2W(H2WA,H2WB),
 O3W(H3WA,H3WB)
3.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C12(H12A,H12B), C18(H18A,H18B), C24(H24A,H24B), C30(H30A,H30B),
 C36(H36A,H36B)
3.c 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(H14A), C15(H15A), C16(H16), C19(H19A), C20(H20A), C21(H21), C22(H22A),
 C25(H25A), C26(H26A), C27(H27A), C28(H28A), C31(H31), C32(H32), C33(H33),
 C34(H34)
;
_shelx_res_checksum              525
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'