Effect of Spacer Atoms in the Dicarboxylate Linkers on the Formation of Coordination Architectures—Molecular Rectangles vs 1D Coordination Polymers: Synthesis, Crystal Structures, Vapor/Gas Adsorption Studies, and Magnetic Properties
Khullar, Sadhika; Mandal, Sanjay K.; Crystal Growth & Design 14 (2014) 6433–; doi:10.1021/cg501284y

data_4512232
_publ_section_title
;
 Effect of Spacer Atoms in the Dicarboxylate Linkers on the Formation of
 Coordination Architectures---Molecular Rectangles vs 1D Coordination
 Polymers: Synthesis, Crystal Structures, Vapor/Gas Adsorption Studies,
 and Magnetic Properties
;
_journal_issue                   12
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              6433
_journal_paper_doi               10.1021/cg501284y
_journal_volume                  14
_journal_year                    2014
_chemical_formula_moiety         'C64 H80 Cu4 N12 O12 S2, 4(Cl O4), 4(H2 O)'
_chemical_formula_sum            'C64 H88 Cl4 Cu4 N12 O32 S2'
_chemical_formula_weight         1997.54
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.6239(16)
_cell_length_b                   20.840(2)
_cell_length_c                   24.643(3)
_cell_measurement_reflns_used    5029
_cell_measurement_temperature    150.(2)
_cell_measurement_theta_max      19.4719
_cell_measurement_theta_min      2.3209
_cell_volume                     8023.8(15)
_computing_cell_refinement       'SAINT V7.68A (Bruker AXS, 2009)'
_computing_data_collection       'APEX2 (Bruker)'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_molecular_graphics    'SHELXTL (Bruker AXS)'
_computing_publication_material  'SHELXTL (Bruker AXS)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker Kappa APEX II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0943
_diffrn_reflns_av_sigmaI/netI    0.0730
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            49533
_diffrn_reflns_theta_full        25.12
_diffrn_reflns_theta_max         25.12
_diffrn_reflns_theta_min         1.65
_diffrn_source                   'sealed tube'
_diffrn_source_type              'fine focus'
_exptl_absorpt_coefficient_mu    1.324
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6525
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.654
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4112
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.018
_refine_diff_density_min         -0.889
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     526
_refine_ls_number_reflns         7079
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.1514
_refine_ls_R_factor_gt           0.0971
_refine_ls_shift/su_max          0.049
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[\s^2^(Fo^2^)+(0.1085P)^2^+72.9691P]
where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2443
_refine_ls_wR_factor_ref         0.2725
_reflns_number_gt                4471
_reflns_number_total             7079
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg501284y_si_002.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 4512230--4512232.cif.'
_cod_database_code               4512232