Controlled Triol-Derivative Bonding and Decoration Transformation on Cu-Centered Anderson-Evans Polyoxometalates.
Wang, Yang; Li, Bao; Qian, Hujun; Wu, Lixin; Inorganic chemistry 55 (2016) 4271–4277; doi:10.1021/acs.inorgchem.6b00008

data_4347319
_publ_section_title
;
 Controlled Triol-Derivative Bonding and Decoration Transformation on
 Cu-Centered Anderson-Evans Polyoxometalates.
;
_journal_issue                   9
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4271
_journal_page_last               4277
_journal_paper_doi               10.1021/acs.inorgchem.6b00008
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C12 H24 Cu Mo6 O24, 2(C16 H36 N), 4(C2 H3 N)'
_chemical_formula_sum            'C52 H108 Cu Mo6 N6 O24'
_chemical_formula_weight         1840.62
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 95.04(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.673(3)
_cell_length_b                   19.662(4)
_cell_length_c                   13.762(3)
_cell_measurement_reflns_used    29747
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.02
_cell_volume                     3685.5(14)
_computing_cell_refinement       RAPID-AUTO
_computing_data_collection       'RAPID-AUTO (Rigaku Corporation, 1998)'
_computing_data_reduction
'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       '\w 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  0.0306
_diffrn_reflns_av_sigmaI/netI    0.0266
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            34490
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    1.343
_exptl_absorpt_correction_T_max  0.8664
_exptl_absorpt_correction_T_min  0.8343
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.659
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1870
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.225
_refine_diff_density_min         -0.545
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         8390
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0328
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0538P)^2^+2.4068P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0900
_refine_ls_wR_factor_ref         0.0946
_reflns_number_gt                7107
_reflns_number_total             8390
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b00008_si_002.cif
_cod_data_source_block           2a
_cod_original_cell_volume        3685.5(13)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4347319