Synthesis and proton conductivity of two novel molybdate polymers
Xu, Li; Wang, Zhifang; Lu, Ying; Yan, Tingting; Tian, Hongrui; Li, Xiaohui; Wang, Shuang; Sun, Xiuwei; Zhang, Zhong; Dang, Tianyi; Liu, Shuxia; New Journal of Chemistry 42 (2018) 16516–; doi:10.1039/C8NJ03781G

data_7057691
_publ_section_title
;
 Synthesis and proton conductivity of two novel molybdate polymers
;
_journal_issue                   20
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              16516
_journal_paper_doi               10.1039/C8NJ03781G
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety         'H8 Mo16 Na2 O56, 2(C36 H24 Co N6), 2(H2 O)'
_chemical_formula_sum            'C72 H60 Co2 Mo16 N12 Na2 O58'
_chemical_formula_weight         3720.20
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-08-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-08-12 deposited with the CCDC.
2018-08-16 downloaded from the CCDC.
;
_cell_angle_alpha                89.715(5)
_cell_angle_beta                 88.414(5)
_cell_angle_gamma                74.499(5)
_cell_formula_units_Z            1
_cell_length_a                   11.184(5)
_cell_length_b                   14.349(5)
_cell_length_c                   16.169(5)
_cell_measurement_reflns_used    5383
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.301
_cell_measurement_theta_min      2.300
_cell_volume                     2499.4(16)
_computing_cell_refinement       'SAINT V8.18C (?, 2016)'
_computing_data_reduction        'SAINT V8.18C (?, 2016)'
_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    'SIR2004 (Burla et al.,  2007)'
_diffrn_ambient_temperature      293.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0235
_diffrn_reflns_av_unetI/netI     0.0514
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18627
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         28.354
_diffrn_reflns_theta_min         1.890
_exptl_absorpt_coefficient_mu    2.370
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4807
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1492 before and 0.0623 after correction. The Ratio of minimum to maximum transmission is 0.6446. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.472
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1787
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.601
_refine_diff_density_min         -0.880
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     730
_refine_ls_number_reflns         12304
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0330
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0295P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0685
_refine_ls_wR_factor_ref         0.0752
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9345
_reflns_number_total             12304
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj03781g2.cif
_cod_data_source_block           y
_cod_depositor_comments
'Adding full bibliography for 7057691--7057692.cif.'
_cod_database_code               7057691
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.733
_shelx_estimated_absorpt_t_min   0.600
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Riding coordinates:
 O21(H21A,H21B), O20(H20A,H20B), O29(H29A,H29B)
2.b Aromatic/amide H refined with riding coordinates:
 C27(H27), C28(H28), C29(H29), C31(H31), C36(H36), C35(H35), C34(H34),
 C16(H16), C17(H17), C15(H15), C12(H12), C11(H11), C10(H10), C8(H8), C7(H7),
 C24(H24), C23(H23), C22(H22), C20(H20), C19(H19), C32(H32), C3(H3), C4(H4),
 C5(H5)
;
_shelx_res_checksum              34796
_olex2_submission_special_instructions 'No special instructions were received'