Stoichiometry, temperature, solvent, metal-directed syntheses of metal‒organic frameworks based on flexible V-shaped methylenebis(3,5-dimethylpyrazole) and various aromatic dicarboxylate acids
Guo, Xiang-Guang; Yang, Wen-Bin; Wu, Xiao-Yuan; Zhang, Qi-Kai; Lin, Lang; Yu, RongMin; Lu, Can-Zhong; CrystEngComm 15 (2013) 3654–; doi:10.1039/c3ce00048f

data_7209584
_publ_section_title
;
 Stoichiometry, temperature, solvent, metal-directed syntheses of
 metal--organic frameworks based on flexible V-shaped
 methylenebis(3,5-dimethylpyrazole) and various aromatic dicarboxylate
 acids
;
_journal_issue                   18
_journal_name_full               CrystEngComm
_journal_page_first              3654
_journal_paper_doi               10.1039/c3ce00048f
_journal_volume                  15
_journal_year                    2013
_chemical_formula_sum            'C19 H19 Br2 Co N4 O4.5'
_chemical_formula_weight         594.13
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 119.568(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.639(3)
_cell_length_b                   13.6527(10)
_cell_length_c                   19.0257(14)
_cell_measurement_temperature    293(2)
_cell_volume                     4436.9(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'superNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_av_sigmaI/netI    0.0524
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            8551
_diffrn_reflns_theta_full        72.07
_diffrn_reflns_theta_max         72.07
_diffrn_reflns_theta_min         4.15
_exptl_absorpt_coefficient_mu    10.598
_exptl_absorpt_correction_T_max  0.3628
_exptl_absorpt_correction_T_min  0.2993
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.779
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2352
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.670
_refine_diff_density_min         -0.704
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         4305
_refine_ls_number_restraints     117
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0960
_refine_ls_R_factor_gt           0.0646
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0750P)^2^+22.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1609
_refine_ls_wR_factor_ref         0.1786
_reflns_number_gt                2960
_reflns_number_total             4305
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce00048f.txt
_cod_data_source_block           a1
_cod_original_cell_volume        4436.9(8)
_cod_original_sg_symbol_H-M      c2/c
_cod_original_formula_sum        'C19 H19 Br2 Co N4 O4.50'
_cod_database_code               7209584