Novel Two-Dimensional Network Constructed from Polyoxomolybdate Chains Linked through Copper−Organonitrogen Coordination Polymer Chains: Hydrothermal Synthesis and Structure of [H2bpy][Cu(4,4‘-bpy)]2[HPCuMo11O39]
Lu, Ying; Xu, Yan; Wang, Enbo; Lü, Jian; Hu, Changwen; Xu, Lin; Crystal Growth & Design 5 (2005) 257–; doi:10.1021/cg0498960

data_4505061
_publ_section_title
;
 Novel Two-Dimensional Network Constructed from Polyoxomolybdate Chains
 Linked through Copper&#x2212;Organonitrogen Coordination Polymer
 Chains:&#x2009; Hydrothermal Synthesis and Structure of
 [H2bpy][Cu(4,4&#x2018;-bpy)]2[HPCuMo11O39]
;
_journal_issue                   1
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              257
_journal_paper_doi               10.1021/cg0498960
_journal_volume                  5
_journal_year                    2005
_chemical_formula_sum            'C30 H27 Cu3 Mo11 N6 O39 P'
_chemical_formula_weight         2372.50
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                96.91(3)
_cell_angle_beta                 110.33(3)
_cell_angle_gamma                103.73(3)
_cell_formula_units_Z            1
_cell_length_a                   10.781(2)
_cell_length_b                   10.885(2)
_cell_length_c                   12.781(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1332.0(6)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID IP diffractometer'
_diffrn_measurement_method       'Oscillation 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0230
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9582
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    3.806
_exptl_absorpt_correction_T_max  0.671
_exptl_absorpt_correction_T_min  0.444
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.956
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1124
_exptl_crystal_size_max          0.225
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.105
_refine_diff_density_max         2.071
_refine_diff_density_min         -2.011
_refine_diff_density_rms         0.470
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.71(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     848
_refine_ls_number_reflns         9582
_refine_ls_number_restraints     478
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0580
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1102P)^2^+14.7510P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1606
_refine_ls_wR_factor_ref         0.1714
_reflns_number_gt                8952
_reflns_number_total             9582
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg0498960si20040322_073123.cif
_cod_data_source_block           C30H27Cu3Mo11N6O39P
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1332.0(5)
_cod_original_sg_symbol_H-M      P1
_cod_database_code               4505061