Spontaneous resolution of non-centrosymmetric coordination polymers of zinc(II) with achiral imidazole-biphenyl-carboxylate ligands
Bejan, Dana; Bahrin, Lucian Gabriel; Shova, Sergiu; Sardaru, Monica; Clima, Lilia; Nicolescu, Alina; Marangoci, Narcisa; Lozan, Vasile; Janiak, Christoph; Inorganica Chimica Acta 482 (2018) 275–283; doi:10.1016/j.ica.2018.05.024

data_1563936
_publ_section_title
;
 Spontaneous resolution of non-centrosymmetric coordination polymers of
 zinc(II) with achiral imidazole-biphenyl-carboxylate ligands
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              275
_journal_page_last               283
_journal_paper_doi               10.1016/j.ica.2018.05.024
_journal_volume                  482
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_moiety         '0.5(C64 H44 N8 O8 Zn2)'
_chemical_formula_sum            'C32 H22 N4 O4 Zn'
_chemical_formula_weight         591.91
_space_group_crystal_system      orthorhombic
_space_group_IT_number           41
_space_group_name_Hall           'A 2 -2ab'
_space_group_name_H-M_alt        'A e a 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.9969(18)
_cell_length_b                   21.6823(19)
_cell_length_c                   7.5937(9)
_cell_measurement_reflns_used    1437
_cell_measurement_temperature    200.05(10)
_cell_measurement_theta_max      26.3210
_cell_measurement_theta_min      1.8670
_cell_volume                     2633.9(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.05(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0797
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -94.00 -38.00   1.00   30.00    --  -23.85-178.00  60.00   56
  2  \w    -35.00  21.00   1.00   30.00    --   26.19 -57.00 -90.00   56
  3  \w    -40.00  16.00   1.00   30.00    --   26.19 -57.00  30.00   56
  4  \w     38.00  78.00   1.00   30.00    --   26.04  57.00 150.00   40
  5  \w     33.00  67.00   1.00   30.00    --   26.04  57.00 120.00   34
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0322611000
_diffrn_orient_matrix_UB_12      -0.0170616000
_diffrn_orient_matrix_UB_13      -0.0416184000
_diffrn_orient_matrix_UB_21      -0.0047142000
_diffrn_orient_matrix_UB_22      0.0237632000
_diffrn_orient_matrix_UB_23      -0.0635340000
_diffrn_orient_matrix_UB_31      0.0300929000
_diffrn_orient_matrix_UB_32      -0.0145820000
_diffrn_orient_matrix_UB_33      -0.0544012000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_unetI/netI     0.0600
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            5019
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.88
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.980
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62888
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.467
_refine_diff_density_min         -0.554
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         2094
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0525
_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^)+(0.0544P)^2^+1.6957P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1114
_refine_ls_wR_factor_ref         0.1154
_reflns_number_gt                1887
_reflns_number_total             2094
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2018-482-275.cif
_cod_data_source_block           shi_3690_dabe
_cod_original_sg_symbol_Hall     'A 2 -2ac'
_cod_database_code               1563936
_chemical_oxdiff_formula         C30H30N6O4Zn1
_chemical_oxdiff_usercomment     ZnL1(2)
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C9(H9), C10(H10), C12(H12), C13(H13),
 C14(H14), C15(H15), C16(H16)
;