Synthesis and properties of four coordination polymers built from a semi-rigid tripod carboxylic acid
Zhou, Lian; Zhang, Jun; Li, Yi-Zhi; Du, Hong-Bin; CrystEngComm 15 (2013) 8989–; doi:10.1039/c3ce41186a

data_7211060
_publ_section_title
;
 Synthesis and properties of four coordination polymers built from a
 semi-rigid tripod carboxylic acid
;
_journal_issue                   44
_journal_name_full               CrystEngComm
_journal_page_first              8989
_journal_paper_doi               10.1039/c3ce41186a
_journal_volume                  15
_journal_year                    2013
_chemical_formula_sum            'C81 H96 Mn3 N5 O26.5'
_chemical_formula_weight         1728.46
_chemical_name_systematic
; 
 ? 
;
_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           SHELXL-97
_cell_angle_alpha                112.451(2)
_cell_angle_beta                 93.548(3)
_cell_angle_gamma                104.215(2)
_cell_formula_units_Z            2
_cell_length_a                   16.1796(15)
_cell_length_b                   19.1505(17)
_cell_length_c                   19.5848(12)
_cell_measurement_reflns_used    7098
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      22.33
_cell_measurement_theta_min      2.20
_cell_volume                     5353.9(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0079
_diffrn_reflns_av_sigmaI/netI    0.0738
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            42686
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    0.411
_exptl_absorpt_correction_T_max  0.9103
_exptl_absorpt_correction_T_min  0.9068
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS;Bruker,2000
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.072
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombus
_exptl_crystal_F_000             1796
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.24
_platon_squeeze_details
;
 Because of the highly disordered solvent molecules, the PLATON/SQUEEZE
 route was employed to calculate the diffraction contribution from the
 solvent molecules, and thereby to produce a set of solvent-free
 diffraction intensities used for refinement. The unit cell was found
 to contain a void of 2260 A^3 (42.2% of the unit cell volume), holding
 113 electrons. These might correspond with the removal of 2 DMF
 and 3 H2O molecules from the unit cell, i.e. 1 DMF and 1.5 H2O 
 per asymmetric unit. Based on the elemental analysis and TG analysis,
 additional 2 DMF might be adsorbed in the sample and were thus
 included in the final molecular formula. Those solvents are included
 in the reported chemical formula and derived values (reported
 crystal-data formula, formula weight, Dx, Mu and F(000)).
;
_refine_diff_density_max         0.842
_refine_diff_density_min         -1.058
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     890
_refine_ls_number_reflns         20816
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0567
_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^)+(0.0600P)^2^+1.8800P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1545
_refine_ls_wR_factor_ref         0.1560
_reflns_number_gt                13118
_reflns_number_total             20816
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce41186a.txt
_cod_data_source_block           2
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'P-1   '
_cod_database_code               7211060