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_7236265
_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 H40 Mo8 N8 Ni2 O28'
_chemical_formula_sum            'C36 H40 Mo8 N8 Ni2 O28'
_chemical_formula_weight         1917.59
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     direct
_audit_creation_date             2016-10-20
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2016.10.10 svn.r3347 for OlexSys, GUI svn.r5252)
;
_audit_update_record
;
2016-10-21 deposited with the CCDC.
2016-11-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.489(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.2553(4)
_cell_length_b                   15.3666(4)
_cell_length_c                   15.4604(5)
_cell_measurement_reflns_used    3686
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.7770
_cell_measurement_theta_min      3.2300
_cell_volume                     2727.35(16)
_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  'olex2.refine (Bourhis et al., 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 0.9988
_diffrn_measured_fraction_theta_max 0.9988
_diffrn_measurement_details
;
  1 omega   22.00   48.35   0.8500    7.5000
omega____ theta____ kappa____ phi______ frames
    -       18.4428   57.0000  -90.0000 31

  2 omega    2.00   78.50   0.8500    7.5000
omega____ theta____ kappa____ phi______ frames
    -       18.4428   57.0000 -180.0000 90

  3 omega  -12.00   21.15   0.8500    7.5000
omega____ theta____ kappa____ phi______ frames
    -       18.4428   83.0000 -103.8659 39

  4 omega  -49.00   45.35   0.8500    7.5000
omega____ theta____ kappa____ phi______ frames
    -       18.4428  -77.0000   30.0000 111
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0164884000
_diffrn_orient_matrix_UB_12      -0.0334794000
_diffrn_orient_matrix_UB_13      0.0337018000
_diffrn_orient_matrix_UB_21      0.0303185000
_diffrn_orient_matrix_UB_22      0.0309032000
_diffrn_orient_matrix_UB_23      0.0339920000
_diffrn_orient_matrix_UB_31      -0.0512317000
_diffrn_orient_matrix_UB_32      0.0075007000
_diffrn_orient_matrix_UB_33      0.0103118000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_unetI/netI     0.0472
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12597
_diffrn_reflns_theta_full        24.9976
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.81
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.540
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96672
_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    2.3349
_exptl_crystal_description       block
_exptl_crystal_F_000             1830.6232
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.6401
_refine_diff_density_min         -0.6510
_refine_diff_density_rms         0.1465
_refine_ls_d_res_high            0.8409
_refine_ls_d_res_low             7.2412
_refine_ls_goodness_of_fit_ref   1.0559
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    36
_refine_ls_number_parameters     369
_refine_ls_number_reflns         4794
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0559
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0292
_refine_ls_shift/su_max          0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0265P)^2^+2.1735P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0634
_refine_ls_wR_factor_ref         0.0692
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              9
_reflns_limit_h_min              -14
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              18
_reflns_limit_l_min              -8
_reflns_number_gt                3996
_reflns_number_total             4794
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c6ra21603j2.cif
_cod_data_source_block           4
_cod_original_cell_volume        2727.36(15)
_cod_database_code               7236265
_chemical_oxdiff_formula         'Ni1 C18 N4 H18 N2 Mo7 O24'
_reflns_odcompleteness_completeness 99.83
_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, All O(H,H) groups
2.a Riding coordinates:
 O1W(H1Wa,H1Wb)
2.b Secondary CH2 refined with riding coordinates:
 C6(H6a,H6b), C12(H12a,H12b), C18(H18a,H18b)
2.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C16(H16), C2(H2), C4(H4), C7(H7), C13(H13), C3(H3), C14(H14), C8(H8),
 C9(H9), C15(H15), C10(H10)
;
_olex2_submission_special_instructions 'No special instructions were received'