Anion-Directed Crystallization of Coordination Polymers: Syntheses and Characterization of Cu4(2-pzc)4(H2O)8(Mo8O26).2H2O and Cu3(2-pzc)4(H2O)2(V10O28H4).6.5H2O (2-pzc = 2-Pyrazinecarboxylate)
Li-Min Zheng; Yongsheng Wang; Xiqu Wang; James D. Korp; Allan J. Jacobson; Inorganic Chemistry 40 (2001) 1380–1385; doi:10.1021/ic0011967

data_4319426
_publ_section_title
;
 Anion-Directed Crystallization of Coordination Polymers: Syntheses and
 Characterization of Cu4(2-pzc)4(H2O)8(Mo8O26).2H2O and
 Cu3(2-pzc)4(H2O)2(V10O28H4).6.5H2O (2-pzc = 2-Pyrazinecarboxylate)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1380
_journal_page_last               1385
_journal_paper_doi               10.1021/ic0011967
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C20 H32 Cu4 Mo8 N8 O44'
_chemical_formula_weight         2110.22
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 90.8160(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.1547(5)
_cell_length_b                   13.4149(6)
_cell_length_c                   15.9633(7)
_cell_measurement_reflns_used    5652
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.51
_cell_measurement_theta_min      1.98
_cell_volume                     2388.49(18)
_computing_cell_refinement       'Bruker SAINT software (Bruker, 1999)'
_computing_data_collection       'Siemens SMART software (Siemens, 1996)'
_computing_data_reduction        'Bruker SAINT software (Bruker, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 1K
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       CCD
_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  0.0322
_diffrn_reflns_av_sigmaI/netI    0.0224
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            11028
_diffrn_reflns_theta_max         23.51
_diffrn_reflns_theta_min         1.98
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    3.898
_exptl_absorpt_correction_T_max  0.840
_exptl_absorpt_correction_T_min  0.631
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.934
_exptl_crystal_description       block
_exptl_crystal_F_000             2024
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.385
_refine_diff_density_min         -0.420
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       0.00026(5)
_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_all   0.996
_refine_ls_goodness_of_fit_obs   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         3529
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      0.995
_refine_ls_restrained_S_obs      1.060
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_obs          0.0218
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0335P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0534
_refine_ls_wR_factor_obs         0.0512
_reflns_number_observed          2936
_reflns_number_total             3711
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0011967_1.cif
_cod_data_source_block           Cu4(2-pzc)4(H2O)8(Mo8O26).2H2O
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0335P)^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^)+(0.0335P)^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        2388.5(2)
_cod_database_code               4319426