Self-assembly and thermotropic liquid crystal properties of a hexavacant germanomolybdate: [Ge2Mo16O58]12−
Gao, Yan-Qing; Zhang, Zhi-Ming; Shen, Jian-Qiang; Jia, Yue; Liu, Zhu-Jun; Wang, En-Bo; CrystEngComm 16 (2014) 6784–; doi:10.1039/c4ce00536h

data_7216182
_publ_section_title
;
 Self-assembly and thermotropic liquid crystal properties of a hexavacant
 germanomolybdate: [Ge2Mo16O58]12&#x2212;
;
_journal_issue                   29
_journal_name_full               CrystEngComm
_journal_page_first              6784
_journal_paper_doi               10.1039/c4ce00536h
_journal_volume                  16
_journal_year                    2014
_chemical_formula_sum            'C9 H66 Ge2 K2 Mo16 N6 O71'
_chemical_formula_weight         3153.09
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 111.10(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.552(5)
_cell_length_b                   17.135(3)
_cell_length_c                   19.302(4)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.450
_cell_measurement_theta_min      3.050
_cell_volume                     7576(3)
_computing_cell_refinement       auto
_computing_data_collection       auto
_computing_data_reduction        auto
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0.01
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID IP'
_diffrn_measurement_method       Oscillation
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0585
_diffrn_reflns_av_unetI/netI     0.0506
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            35236
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.450
_diffrn_reflns_theta_min         3.050
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.560
_exptl_absorpt_correction_T_max  0.457
_exptl_absorpt_correction_T_min  0.412
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR by T.Higashi    8 March, 1995'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.765
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6016
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.220
_refine_diff_density_max         2.291
_refine_diff_density_min         -0.955
_refine_diff_density_rms         0.220
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         8633
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0464
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1000P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1322
_refine_ls_wR_factor_ref         0.1440
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6667
_reflns_number_total             8633
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4ce00536h2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7216182--7216183.cif.'
_cod_database_code               7216182
_shelx_estimated_absorpt_t_min   0.458
_shelx_estimated_absorpt_t_max   0.508
_shelxl_version_number           2013-2
_shelx_res_checksum              2368