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_7057692
_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         'Mo4 O13, 3(H2 O), C6 H14 N2'
_chemical_formula_sum            'C6 H20 Mo4 N2 O16'
_chemical_formula_weight         760.00
_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     dual
_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                66.2630(10)
_cell_angle_beta                 83.398(2)
_cell_angle_gamma                86.412(2)
_cell_formula_units_Z            2
_cell_length_a                   7.9489(8)
_cell_length_b                   10.7707(11)
_cell_length_c                   11.6957(13)
_cell_measurement_reflns_used    4228
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      28.349
_cell_measurement_theta_min      2.580
_cell_volume                     910.40(17)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0157
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6594
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.374
_diffrn_reflns_theta_min         1.911
_exptl_absorpt_coefficient_mu    2.777
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4251
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1584 before and 0.0637 after correction. The Ratio of minimum to maximum transmission is 0.5701. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.772
_exptl_crystal_description       block
_exptl_crystal_F_000             732
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.546
_refine_diff_density_min         -0.731
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         4498
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0257
_refine_ls_R_factor_gt           0.0212
_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^)+(0.0226P)^2^+0.0704P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0518
_refine_ls_wR_factor_ref         0.0533
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4014
_reflns_number_total             4498
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj03781g2.cif
_cod_data_source_block           w
_cod_depositor_comments
'Adding full bibliography for 7057691--7057692.cif.'
_cod_database_code               7057692
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.750
_shelx_estimated_absorpt_t_min   0.607
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Riding coordinates:
 O15(H15A,H15B), O16(H16A,H16B)
2.b Free rotating group:
 O14(H14A,H14B)
2.c Ternary CH refined with riding coordinates:
 N1(H1), N2(H2)
2.d Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B)
;
_shelx_res_checksum              27634
_olex2_submission_special_instructions 'No special instructions were received'