Increasing nuclearity of secondary building units in porous cobalt(ii) metal-organic frameworks: Variation in structure and H(2) adsorption.
Jia, Junhua; Athwal, Harprit Singh; Blake, Alexander J.; Champness, Neil R.; Hubberstey, Peter; Schröder, Martin; Dalton transactions (Cambridge, England : 2003) 40 (2011) 12342–12349; doi:10.1039/c1dt10901d

data_7017274
_publ_section_title
;
 Increasing nuclearity of secondary building units in porous cobalt(ii)
 metal-organic frameworks: Variation in structure and H(2) adsorption.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12342
_journal_page_last               12349
_journal_paper_doi               10.1039/c1dt10901d
_journal_volume                  40
_journal_year                    2011
_chemical_formula_moiety         'C40.5 H27.5 Co3 N3.5 O14, 6.75(C3 H7 N O)'
_chemical_formula_sum            'C60.75 H74.75 Co3 N10.25 O20.75'
_chemical_formula_weight         1457.35
_space_group_IT_number           2
_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           SHELXL97
_cell_angle_alpha                86.833(9)
_cell_angle_beta                 80.346(8)
_cell_angle_gamma                83.224(9)
_cell_formula_units_Z            2
_cell_length_a                   10.164(6)
_cell_length_b                   13.363(8)
_cell_length_c                   22.395(13)
_cell_measurement_reflns_used    2206
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      22.9
_cell_measurement_theta_min      2.29
_cell_volume                     2976(3)
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       omega
_diffrn_radiation_monochromator  'silicon (111)'
_diffrn_radiation_source         'Daresbury Laboratory Station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6902
_diffrn_reflns_av_R_equivalents  0.101
_diffrn_reflns_av_sigmaI/netI    0.173
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            22034
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    0.920
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.465
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS v2.03'
_exptl_crystal_colour            PURPLE
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       LATH
_exptl_crystal_F_000             1516
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
The results above correspond to 271 electrons/Co3 or 6.75 lattice
DMF/Co3 in unit cell. These molecules have been included
in the formula.

Coordinated DMF molecule was treated as half-occupancy, sharing an O atoms
with a half-occupied water molecule. The H atoms of these molecules cannot
be located, but have been included in the formula.

The C-O11, C-O11 and C-O12 distances were restrained.
;
_refine_diff_density_max         1.02
_refine_diff_density_min         -0.70
_refine_diff_density_rms         0.13
_refine_ls_extinction_coef       0.0097(11)
_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   0.84
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         10100
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.84
_refine_ls_R_factor_all          0.138
_refine_ls_R_factor_gt           0.0799
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
calc w=1/[\s^2^(Fo^2^)+(0.1204P)^2^] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.203
_refine_ls_wR_factor_ref         0.224
_reflns_number_gt                4437
_reflns_number_total             10100
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            c1dt10901d.txt
_cod_data_source_block           compound_3
_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        2975(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7017274