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_1563933
_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_formula_moiety         'C9 H7 I N2'
_chemical_formula_sum            'C9 H7 I N2'
_chemical_formula_weight         270.07
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.1493(7)
_cell_length_b                   8.2568(7)
_cell_length_c                   21.3201(13)
_cell_measurement_reflns_used    2039
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      31.9460
_cell_measurement_theta_min      1.9610
_cell_volume                     1786.6(2)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0797
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -79.00 -48.00   1.00    2.00    --  -24.16-178.00-180.00   31
  2  \w    -81.00 -43.00   1.00    2.00    --  -24.16 -58.00  16.00   38
  3  \w    -45.00  46.00   1.00    2.00    --   26.35 -19.00  30.00   91
;
_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      0.0024346000
_diffrn_orient_matrix_UB_12      -0.0372322000
_diffrn_orient_matrix_UB_13      0.0299471000
_diffrn_orient_matrix_UB_21      0.0483425000
_diffrn_orient_matrix_UB_22      0.0567572000
_diffrn_orient_matrix_UB_23      0.0097341000
_diffrn_orient_matrix_UB_31      -0.0504219000
_diffrn_orient_matrix_UB_32      0.0526199000
_diffrn_orient_matrix_UB_33      0.0107463000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_unetI/netI     0.0466
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            4310
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.77
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.527
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.22387
_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    2.008
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.230
_refine_diff_density_min         -1.780
_refine_diff_density_rms         0.216
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         1572
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0472
_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^)+(0.0774P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1213
_refine_ls_wR_factor_ref         0.1289
_reflns_number_gt                1336
_reflns_number_total             1572
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2018-482-275.cif
_cod_data_source_block           shi_3579_beda
_cod_database_code               1563933
_reflns_odcompleteness_completeness 99.97
_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:
 C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9)
;