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_7211062
_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            'C78 H94 N4 O28 Zn3'
_chemical_formula_weight         1726.39
_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                115.514(2)
_cell_angle_beta                 96.834(3)
_cell_angle_gamma                108.036(2)
_cell_formula_units_Z            2
_cell_length_a                   14.692(2)
_cell_length_b                   18.436(3)
_cell_length_c                   19.8419(16)
_cell_measurement_reflns_used    9910
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.33
_cell_volume                     4408.0(10)
_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, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0171
_diffrn_reflns_av_sigmaI/netI    0.0620
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            35408
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.34
_exptl_absorpt_coefficient_mu    0.886
_exptl_absorpt_correction_T_max  0.8379
_exptl_absorpt_correction_T_min  0.8113
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS;Bruker,2000
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_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 1225 A^3 (28.8% of the unit cell volume), holding
 59 electrons. These might correspond with the removal of ~6 H2O
 molecules from the unit cell, i.e. 3 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         0.708
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     911
_refine_ls_number_reflns         17137
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0546
_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^+1.9900P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1376
_refine_ls_wR_factor_ref         0.1383
_reflns_number_gt                12773
_reflns_number_total             17137
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce41186a.txt
_cod_data_source_block           4
_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_cell_volume        4407.8(9)
_cod_original_sg_symbol_H-M      'P-1   '
_cod_database_code               7211062