Two new helical compounds based on Keggin clusters and N-donor multidentate ligand: Syntheses, structures and properties
Zhou, Shi; Liu, Bo; Li, Xiao-Min; Shi, Tian; Chen, Ya-Guang; Journal of Solid State Chemistry 219 (2014) 15–20; doi:10.1016/j.jssc.2014.07.005

data_1562215
_publ_section_title
;
 Two new helical compounds based on Keggin clusters and N-donor
 multidentate ligand: Syntheses, structures and properties
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              15
_journal_page_last               20
_journal_paper_doi               10.1016/j.jssc.2014.07.005
_journal_volume                  219
_journal_year                    2014
_chemical_formula_moiety         'C36 H33 Cu Ge Mo12 N10 O42'
_chemical_formula_sum            'C36 H33 Cu Ge Mo12 N10 O42'
_chemical_formula_weight         2565.13
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.5290(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.8681(6)
_cell_length_b                   15.1661(6)
_cell_length_c                   24.9681(10)
_cell_measurement_reflns_used    8612
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.38
_cell_measurement_theta_min      2.43
_cell_volume                     5990.0(4)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'APEX2 (Bruker, 2002)'
_computing_data_reduction        'SAINT (Bruker, 2002)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0195
_diffrn_reflns_av_sigmaI/netI    0.0223
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            32129
_diffrn_reflns_theta_full        26.06
_diffrn_reflns_theta_max         26.06
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    3.376
_exptl_absorpt_correction_T_max  0.5402
_exptl_absorpt_correction_T_min  0.2789
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2002)'
_exptl_crystal_colour            'brownish red'
_exptl_crystal_density_diffrn    2.844
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4880
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.034
_refine_diff_density_min         -0.660
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     919
_refine_ls_number_reflns         11806
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0242
_refine_ls_R_factor_gt           0.0204
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0233P)^2^+7.3670P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0498
_refine_ls_wR_factor_ref         0.0513
_reflns_number_gt                10745
_reflns_number_total             11806
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            JSSC-2014-219-15.cif
_cod_data_source_block           GeMo12
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               1562215