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_1562216
_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_sum            'C36 H33 Cu Mo12 N10 O42 Si'
_chemical_formula_weight         2520.63
_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                 94.514(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.864(3)
_cell_length_b                   15.159(3)
_cell_length_c                   25.011(5)
_cell_measurement_reflns_used    8452
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.19
_cell_measurement_theta_min      2.38
_cell_volume                     5996(2)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'APEX2 (Bruker, 2002)'
_computing_data_reduction        'SAINT (Bruker, 2002)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0240
_diffrn_reflns_av_sigmaI/netI    0.0285
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            32309
_diffrn_reflns_theta_full        26.06
_diffrn_reflns_theta_max         26.06
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    2.901
_exptl_absorpt_correction_T_max  0.7222
_exptl_absorpt_correction_T_min  0.4215
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2002)'
_exptl_crystal_colour            'brownish red'
_exptl_crystal_density_diffrn    2.792
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4808
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.907
_refine_diff_density_min         -0.688
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     919
_refine_ls_number_reflns         11797
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0283
_refine_ls_R_factor_gt           0.0221
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0221P)^2^+6.2859P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0502
_refine_ls_wR_factor_ref         0.0525
_reflns_number_gt                10303
_reflns_number_total             11797
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            JSSC-2014-219-15.cif
_cod_data_source_block           SiMo12
_cod_original_cell_volume        5996.2(19)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               1562216