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_7211059
_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            'C75 H83 Cd3 N3 O25'
_chemical_formula_weight         1763.7
_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                65.774(2)
_cell_angle_beta                 87.413(3)
_cell_angle_gamma                67.535(2)
_cell_formula_units_Z            2
_cell_length_a                   14.7676(18)
_cell_length_b                   19.2240(14)
_cell_length_c                   19.7451(16)
_cell_measurement_reflns_used    3580
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      0.852
_cell_measurement_theta_min      0.816
_cell_volume                     4682.3(8)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0148
_diffrn_reflns_av_sigmaI/netI    0.0753
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            28581
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.14
_exptl_absorpt_coefficient_mu    0.740
_exptl_absorpt_correction_T_max  0.8562
_exptl_absorpt_correction_T_min  0.8220
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS;Bruker,2000
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1796
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_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 1892 A^3 (40.1% of the unit cell volume), holding
 120 electrons. These might correspond with the removal of ~3 DMF
 molecules from the unit cell, i.e. 1.5 DMF per asymmetric unit. Based
 on the elemental analysis and TG analysis, additional 1.5 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         1.470
_refine_diff_density_min         -1.045
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     825
_refine_ls_number_reflns         18313
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0528
_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^)+(0.0700P)^2^+1.9900P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1665
_refine_ls_wR_factor_ref         0.1671
_reflns_number_gt                9634
_reflns_number_total             18313
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce41186a.txt
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7211059