Influence of Angular Dicarboxylate Ligand on the Structures of Single and Double Pillared-Layer Coordination Polymers of Co(II)
Park, In-Hyeok; Medishetty, Raghavender; Lee, Hyeong-Hwan; Herng, Tun Seng; Ding, Jun; Lee, Shim Sung; Vittal, Jagadese J.; Crystal Growth & Design 15 (2015) 4156–; doi:10.1021/acs.cgd.5b00766

data_4513444
_publ_section_title
;
 Influence of Angular Dicarboxylate Ligand on the Structures of Single and
 Double Pillared-Layer Coordination Polymers of Co(II)
;
_journal_issue                   8
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              4156
_journal_paper_doi               10.1021/acs.cgd.5b00766
_journal_volume                  15
_journal_year                    2015
_chemical_formula_sum            'C68 H48 Co2 N4 O10'
_chemical_formula_weight         1198.96
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 108.127(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.9388(13)
_cell_length_b                   9.2136(6)
_cell_length_c                   26.536(2)
_cell_measurement_reflns_used    8946
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.21
_cell_measurement_theta_min      2.29
_cell_volume                     4168.2(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0708
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            62023
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         1.615
_exptl_absorpt_coefficient_mu    0.443
_exptl_absorpt_correction_T_max  0.937
_exptl_absorpt_correction_T_min  0.857
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2010)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    0.955
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1236
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.150
_platon_squeeze_details
;
 The TG showed large weight loss due to the presence of DMF
 and water. But in the least square refinements they were
 not located. Further PLATON showed 1305.3 A^3 total solvent
 accessible void which account for 31.3% of the volume of 
 the unit cell. Hence the data were SQUEEZEed to remove 
 the electron densities in the solvent regions. The electron
 count/cell = 473.
 Ref: Sluis, P. v.d. and Spek, A. L. (1990) Acta Cryst. A46, 194-201
;
_refine_diff_density_max         0.798
_refine_diff_density_min         -0.557
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         7764
_refine_ls_number_restraints     238
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0972
_refine_ls_R_factor_gt           0.0785
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1160P)^2^+5.8638P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2128
_refine_ls_wR_factor_ref         0.2251
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5894
_reflns_number_total             7764
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg5b00766_si_002.cif
_cod_data_source_block           ih1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 4513444--4513445.cif.
;
_cod_original_cell_volume        4168.3(5)
_cod_database_code               4513444
_shelx_estimated_absorpt_t_min   0.857
_shelx_estimated_absorpt_t_max   0.937
_platon_squeeze_void_probe_radius 1.20
_shelxl_version_number           2014-3
_shelx_res_checksum              10532
_shelx_hkl_checksum              33580