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_4512231
_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
'C32 H38 Cl Cu2 N6 O10, Cl O4, C2 H3 N, (H2 O)0.5, (H2 O)0.5'
_chemical_formula_sum            'C34 H43 Cl2 Cu2 N7 O15'
_chemical_formula_weight         987.73
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 92.817(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.5695(8)
_cell_length_b                   11.3027(10)
_cell_length_c                   21.867(2)
_cell_measurement_reflns_used    4922
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      24.4940
_cell_measurement_theta_min      2.3795
_cell_volume                     2115.4(3)
_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      100.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0354
_diffrn_reflns_av_sigmaI/netI    0.0756
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            14302
_diffrn_reflns_theta_full        25.08
_diffrn_reflns_theta_max         25.08
_diffrn_reflns_theta_min         0.93
_diffrn_source                   'sealed tube'
_diffrn_source_type              'fine focus'
_exptl_absorpt_coefficient_mu    1.206
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6644
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.389
_refine_diff_density_min         -0.726
_refine_ls_abs_structure_details
;
Flack x determined using 2156 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.039(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         6675
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0695
_refine_ls_R_factor_gt           0.0596
_refine_ls_shift/su_max          0.040
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[\s^2^(Fo^2^)+(0.1180P)^2^+1.7077P]
where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1635
_refine_ls_wR_factor_ref         0.1732
_reflns_number_gt                5855
_reflns_number_total             6675
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg501284y_si_002.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 4512230--4512232.cif.'
_cod_database_code               4512231