A supramolecular Co(II)14-metal-organic cube in a hydrogen-bonded network and a Co(II)-organic framework with a flexible methoxy substituent
Suvendu Sekhar Mondal; Asamanjoy Bhunia; Alexandra Kelling; Uwe Schilde; Christoph Janiak; Hans-Jurgen Holdt; Chem.Commun. 50 (2014) 5441–; doi:10.1039/C3CC49698H

data_7113307
_publ_section_title
;
 A supramolecular Co(II)14-metal-organic cube in a hydrogen-bonded network
 and a Co(II)-organic framework with a flexible methoxy substituent
;
_journal_name_full               Chem.Commun.
_journal_page_first              5441
_journal_paper_doi               10.1039/C3CC49698H
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C8.5 H8.25 Co1.75 N6.5 O5.375, 2(C3 H7 N O)'
_chemical_formula_sum            'C14.5 H22.25 Co1.75 N8.5 O7.375'
_chemical_formula_weight         536.78
_chemical_name_systematic
;
 catena-(dodecakis(\m~3~-4,5-diamide-2-olato-imidazolato)-(\m-~6~oxo)-tetra-
 aqua-dihydroxo-tetradeca-zinc(II)) dimethylformamide solvate
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_Hall           '-I 4'
_space_group_name_H-M_alt        'I 4/m'
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/m'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   17.8029(3)
_cell_length_b                   17.8029(3)
_cell_length_c                   29.2271(7)
_cell_measurement_reflns_used    90084
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.19
_cell_measurement_theta_min      1.34
_cell_volume                     9263.3(3)
_computing_cell_refinement       'X-AREA (Stoe, 2004)'
_computing_data_collection       'X-AREA (Stoe, 2004)'
_computing_data_reduction        'X-RED (Stoe, 2004)'
_computing_publication_material
;
 SHELXL-2013 (Sheldrick, 2013)' 
 TOPOS 4.0 (Blatov, 2006)
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
; 
 180 frames, 7 min exposure time
;
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       '\w scan, \d \w = 1.0 deg'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1056
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            29163
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.339
_exptl_absorpt_coefficient_mu    1.313
_exptl_absorpt_correction_T_max  0.8501
_exptl_absorpt_correction_T_min  0.6144
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'X-Red (Stoe, 2004)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4400
_exptl_crystal_size_max          0.440
_exptl_crystal_size_mid          0.420
_exptl_crystal_size_min          0.400
_refine_diff_density_max         0.916
_refine_diff_density_min         -0.622
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       0.00037(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   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         4156
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0623
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0986P)^2^+23.6803P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1750
_refine_ls_wR_factor_ref         0.1815
_reflns_number_gt                3557
_reflns_number_total             4156
_reflns_threshold_expression     'I > 2\s(I)'
_cod_duplicate_entry             7112265
_cod_data_source_file            c3cc49698h2-1.cif
_cod_data_source_block           suv29
_cod_original_cell_volume        9263.3(4)
_cod_original_formula_sum        'C14.50 H22.25 Co1.75 N8.50 O7.375'
_cod_database_code               7113307