Hydrothermal synthesis and crystal structures of two bimetallic chain-like and cluster complexes [{Co(phen)2}2V6O17]n and [{Cu(phen)2}4V10O29]·6H2O
Zhang, Xian-Ming; Tong, Ming-Liang; Chen, Xiao-Ming; Chemical Communications  (2000) 1817–; doi:10.1039/b005880g

data_7115122
_publ_section_title
;
 Hydrothermal synthesis and crystal structures of two bimetallic
 chain-like and cluster complexes [{Co(phen)2}2V6O17]n and
 [{Cu(phen)2}4V10O29]&#x00B7;6H2O
;
_journal_issue                   18
_journal_name_full               'Chemical Communications'
_journal_page_first              1817
_journal_paper_doi               10.1039/b005880g
_journal_year                    2000
_chemical_formula_sum            'C96 H76 Cu4 N16 O35 V10'
_chemical_formula_weight         2777.29
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_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                 105.81(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.726(3)
_cell_length_b                   14.612(3)
_cell_length_c                   25.310(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      12
_cell_volume                     5240(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT+(Bruker,1999)'
_computing_molecular_graphics    'SHELXTL V.5.0 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'Bruker CCD'
_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  0.0372
_diffrn_reflns_av_sigmaI/netI    0.0702
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            37028
_diffrn_reflns_theta_full        30.05
_diffrn_reflns_theta_max         30.05
_diffrn_reflns_theta_min         3.93
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.730
_exptl_absorpt_correction_T_max  0.917
_exptl_absorpt_correction_T_min  0.745
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.760
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2780
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.873
_refine_diff_density_min         -1.489
_refine_diff_density_rms         0.091
_refine_ls_extinction_coef       0.00000(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.956
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     755
_refine_ls_number_reflns         15179
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      0.956
_refine_ls_R_factor_all          0.1093
_refine_ls_R_factor_gt           0.0522
_refine_ls_shift/su_max          0.091
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0776P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1324
_refine_ls_wR_factor_ref         0.1547
_reflns_number_gt                8042
_reflns_number_total             15179
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b005880g.txt
_cod_data_source_block           complex_2
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0776P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0776P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        5240.1(18)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7115122