Four-connected metal‒organic frameworks constructed by tetracarboxylate acid-based ligands
Sun, Libo; Pan, Qinhe; Liang, Zhiqiang; Yu, Jihong; Inorganic Chemistry Frontiers 1 (2014) 478–; doi:10.1039/c4qi00047a

data_4348212
_publ_section_title
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 Four-connected metal--organic frameworks constructed by tetracarboxylate
 acid-based ligands
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_journal_issue                   6
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              478
_journal_paper_doi               10.1039/c4qi00047a
_journal_volume                  1
_journal_year                    2014
_chemical_formula_sum            'C33 H34 Mn2 N4 O11'
_chemical_formula_weight         772.52
_space_group_IT_number           161
_space_group_name_Hall           'R 3 -2"c'
_space_group_name_H-M_alt        'R 3 c :H'
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   'R 3 c :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            18
_cell_length_a                   38.9881(10)
_cell_length_b                   38.9881(10)
_cell_length_c                   22.2962(11)
_cell_measurement_temperature    296(2)
_cell_volume                     29351.2(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0698
_diffrn_reflns_av_sigmaI/netI    0.0904
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -51
_diffrn_reflns_limit_k_max       51
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            71268
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.04
_exptl_absorpt_coefficient_mu    0.422
_exptl_absorpt_correction_T_max  0.8664
_exptl_absorpt_correction_T_min  0.7860
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   Process-auto
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    0.787
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             7164
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.35
_platon_squeeze_details
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The remaining solvent molecules were disordered and assigned as 36 DMF molecules.
per unit cell, which were determined by TGA, elemental analysis and SQUEEZE results. 
The contributions of these disordered solvents to the scattering values have been removed 
by using the PLATON SQUEEZE program. We can see from the SQUEEZE that some 5745 electrons were 
removed from the unit cell, or some 5745/18 = 319 electrons per formula unit. This total includes 21 electrons 
from the hydrogen of the terminal coordinated DMF molecules in the backbone and other electrons (298 e) from 
disordered solvent, approximately 7.5 DMF (300 e) in the channel. From the calculation and
related information (The CHN and TGA), the formula unit should include 7.5 DMF.
Anal. Calcd for C111H153Mn4N23O37: C, 50.86; H, 5.88; N, 12.29 %; found: C, 48.28; H, 5.75; N, 9.63 %.
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_refine_diff_density_max         0.199
_refine_diff_density_min         -0.171
_refine_diff_density_rms         0.032
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.001(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         16106
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0967
_refine_ls_R_factor_gt           0.0445
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0146P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0680
_refine_ls_wR_factor_ref         0.0730
_reflns_number_gt                8099
_reflns_number_total             16106
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4qi00047a2.cif
_cod_data_source_block           r3c
_cod_depositor_comments
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The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Hexagonal' was changed to
'hexagonal' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
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_cod_original_sg_symbol_H-M      R3c
_cod_database_code               4348212