A square two-dimensional polymer of cobalt citrate cubanes
Falvello, Larry R.; Forcén-Vázquez, Elena; Mayoral, Isabel; Tomás, Milagros; Palacio, Fernando; Acta Crystallographica Section C 67 (2011) m359–m363; doi:10.1107/S0108270111043587

data_2018289
_publ_section_title
;
 A square two-dimensional polymer of cobalt citrate cubanes
;
_journal_coeditor_code           GZ3201
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m359
_journal_page_last               m363
_journal_paper_doi               10.1107/S0108270111043587
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac
'Cs2 [Co (H2 O1)6] [Co6 (C6 H4 O7)4 (H2 O1)8] , 12H2 O'
_chemical_formula_moiety
'2(Cs 1+), C24 H32 Co6 O36 4-, H12 Co O6 2+, 12(H2 O)'
_chemical_formula_sum            'C24 H68 Co7 Cs2 O54'
_chemical_formula_weight         1899.11
_chemical_name_systematic
;
poly[dicaesium(I) hexaaquacobalt(II) [octaaqua-tetra-\m-citrato-hexacobalt(II)]
dodecahydrate]
;
_space_group_IT_number           114
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4 2n'
_symmetry_space_group_name_H-M   'P -4 21 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.57380(10)
_cell_length_b                   12.57380(10)
_cell_length_c                   19.5895(3)
_cell_measurement_reflns_used    8136
_cell_measurement_temperature    100.0(10)
_cell_measurement_theta_max      28.799
_cell_measurement_theta_min      4.153
_cell_volume                     3097.11(6)
_computing_cell_refinement       'CrysAlisPro (Oxford Diffraction, 2010)'
_computing_data_collection       'CrysAlisPro (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlisPro (Oxford Diffraction, 2010)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2005)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, (2007)'
_diffrn_ambient_temperature      100.0(10)
_diffrn_detector_area_resol_mean 16.0655
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_device_type  'Oxford Xcalibur, Sapphire3'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_av_sigmaI/netI    0.0439
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            14807
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.83
_diffrn_reflns_theta_min         4.16
_exptl_absorpt_coefficient_mu    3.106
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79022
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(multi-scan absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm; Oxford Diffraction,
2010)
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    2.036
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             1886
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.582
_refine_diff_density_min         -0.447
_refine_ls_abs_structure_details 'Flack (1983), with how many Friedel pairs?'
_refine_ls_abs_structure_Flack   0.04(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         3677
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0372
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0590P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0918
_refine_ls_wR_factor_ref         0.0935
_reflns_number_gt                3128
_reflns_number_total             3677
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gz3201.cif
_cod_data_source_block           I
_cod_database_code               2018289
_cod_database_fobs_code          2018289