Construction of Chiral [4 + 4] and [2 + 2] Schiff-Base Macrocyclic Zinc(II) Complexes Influenced by Counterions and Pendant Arms.
Hu, Yong; Zhang, Lei; Chang, Fei-Fan; Zhao, Pei-Chen; Feng, Gen-Feng; Zhang, Kun; Huang, Wei; Inorganic chemistry 55 (2016) 8260–8262; doi:10.1021/acs.inorgchem.6b01493

data_4348660
_publ_section_title
;
 Construction of Chiral [4 + 4] and [2 + 2] Schiff-Base Macrocyclic
 Zinc(II) Complexes Influenced by Counterions and Pendant Arms.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8260
_journal_page_last               8262
_journal_paper_doi               10.1021/acs.inorgchem.6b01493
_journal_volume                  55
_journal_year                    2016
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C60 H64 Cl4 N6 O6 Zn2, 4(C2 H6 O), 2(N O3)'
_chemical_formula_sum            'C68 H88 Cl4 N8 O16 Zn2'
_chemical_formula_weight         1546.04
_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_Hall           'P 4nw 2abw'
_space_group_name_H-M_alt        'P 43 21 2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.8383(10)
_cell_length_b                   14.8383(10)
_cell_length_c                   33.384(5)
_cell_measurement_reflns_used    2553
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      17.861
_cell_measurement_theta_min      2.293
_cell_volume                     7350.3(13)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (BRUKER 2000)'
_computing_data_reduction        'SAINT (BRUKER 2000)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (BRUKER 2000)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1336
_diffrn_reflns_av_unetI/netI     0.0913
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            40558
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.996
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         1.836
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.868
_exptl_absorpt_correction_T_max  0.9182
_exptl_absorpt_correction_T_min  0.9030
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker(2000)'
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3232
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.419
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details
;
 Flack x determined using 1448 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.011(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     444
_refine_ls_number_reflns         6475
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0974
_refine_ls_R_factor_gt           0.0517
_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^)+(0.0555P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1043
_refine_ls_wR_factor_ref         0.1177
_reflns_Friedel_coverage         0.728
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                4443
_reflns_number_total             6475
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01493_si_002.cif
_cod_data_source_block           3
_cod_original_cell_volume        7350.4(14)
_cod_database_code               4348660
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.903
_shelx_estimated_absorpt_t_max   0.918
_shelx_res_checksum              15479
_shelx_hkl_checksum              91864