Bifunctional pyrazolate‒carboxylate ligands for isoreticular cobalt and zinc MOF-5 analogs with magnetic analysis of the {Co4(μ4-O)} node
Heering, Christian; Boldog, Ishtvan; Vasylyeva, Vera; Sanchiz, Joaquín; Janiak, Christoph; CrystEngComm 15 (2013) 9757–; doi:10.1039/c3ce41426d

data_7238855
_publ_section_title
;
 Bifunctional pyrazolate--carboxylate ligands for isoreticular cobalt and
 zinc MOF-5 analogs with magnetic analysis of the {Co4(\m4-O)} node
;
_journal_issue                   45
_journal_name_full               CrystEngComm
_journal_page_first              9757
_journal_paper_doi               10.1039/c3ce41426d
_journal_volume                  15
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C18 H18 Co4 N6 O7'
_chemical_formula_sum            'C18 H18 Co4 N6 O7'
_chemical_formula_weight         666.11
_chemical_name_common            HHU-1
_space_group_crystal_system      cubic
_space_group_IT_number           216
_space_group_name_Hall           'F -4 2 3'
_space_group_name_H-M_alt        'F -4 3 m'
_symmetry_space_group_name_Hall  'F -4 2 3'
_symmetry_space_group_name_H-M   'F -4 3 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-08-14
_audit_creation_method
;
  Olex2 1.1-beta
  (compiled 2011.11.01 svn.r2039, GUI svn.r3906)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.1090(7)
_cell_length_b                   20.1090(7)
_cell_length_c                   20.1090(7)
_cell_measurement_reflns_used    526
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      66.2526
_cell_measurement_theta_min      4.3938
_cell_volume                     8131.5(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.2 (release 08-11-2011 CrysAlis171 .NET)
(compiled Nov 15 2011,12:54:45)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.2 (release 08-11-2011 CrysAlis171 .NET)
(compiled Nov 15 2011,12:54:45)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.2 (release 08-11-2011 CrysAlis171 .NET)
(compiled Nov 15 2011,12:54:45)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 5.1734
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
  1 omega  -91.00  -48.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  133.0000   25.0000 43

  2 omega   44.00   71.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      106.4053  -30.0000  120.0000 27

  3 omega   33.00   89.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      106.4053  -30.0000    0.0000 56
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0115050000
_diffrn_orient_matrix_UB_12      0.0023011000
_diffrn_orient_matrix_UB_13      0.0757680000
_diffrn_orient_matrix_UB_21      0.0753513000
_diffrn_orient_matrix_UB_22      -0.0074872000
_diffrn_orient_matrix_UB_23      0.0116468000
_diffrn_orient_matrix_UB_31      0.0075854000
_diffrn_orient_matrix_UB_32      0.0761674000
_diffrn_orient_matrix_UB_33      -0.0009108000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            1559
_diffrn_reflns_theta_full        66.36
_diffrn_reflns_theta_max         66.36
_diffrn_reflns_theta_min         4.40
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.829
_exptl_absorpt_correction_T_max  0.307
_exptl_absorpt_correction_T_min  0.196
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.2 (release 08-11-2011 CrysAlis171 .NET)
(compiled Nov 15 2011,12:54:45)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
;
_exptl_crystal_colour            'blue violet'
_exptl_crystal_density_diffrn    1.088
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             2656
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_platon_squeeze_details
;
The unit cell contains solvent molecules which have been treated 
as a diffuse contribution to the overall scattering without specific 
atom positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         1.341
_refine_diff_density_min         -0.668
_refine_diff_density_rms         0.126
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.42(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     54
_refine_ls_number_reflns         641
_refine_ls_number_restraints     71
_refine_ls_restrained_S_all      1.181
_refine_ls_R_factor_all          0.0814
_refine_ls_R_factor_gt           0.0723
_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^)+(0.1476P)^2^+5.2065P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2078
_refine_ls_wR_factor_ref         0.2203
_reflns_number_gt                503
_reflns_number_total             641
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce41426d.txt
_cod_data_source_block           ibe19
_cod_database_code               7238855
_chemical_oxdiff_formula         'Co4 C18 H18 N6 O7 Cl8 (C O H4)8'
_reflns_odcompleteness_completeness 99.04
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49