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_1563937
_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         'C16 H12 N2 O2'
_chemical_formula_sum            'C16 H12 N2 O2'
_chemical_formula_weight         264.28
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 97.948(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   3.8466(7)
_cell_length_b                   27.589(5)
_cell_length_c                   11.6689(18)
_cell_measurement_reflns_used    1032
_cell_measurement_temperature    200.05(10)
_cell_measurement_theta_max      31.4830
_cell_measurement_theta_min      1.9190
_cell_volume                     1226.5(4)
_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    'SIR2008 (Burla et al., 2007)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega   38.00   64.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       26.1940  -99.0000  -30.0000 52

  2 omega  -24.00   64.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       26.1940  -99.0000 -120.0000 176

  3 omega  -87.00  -54.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.8503  -57.0000   90.0000 66

  4 omega  -90.00  -10.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.8503  -57.0000    0.0000 160
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0279799000
_diffrn_orient_matrix_UB_12      0.0004201000
_diffrn_orient_matrix_UB_13      -0.0613370000
_diffrn_orient_matrix_UB_21      0.0097370000
_diffrn_orient_matrix_UB_22      -0.0256670000
_diffrn_orient_matrix_UB_23      -0.0011020000
_diffrn_orient_matrix_UB_31      -0.1837904000
_diffrn_orient_matrix_UB_32      -0.0014272000
_diffrn_orient_matrix_UB_33      0.0007847000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.0880
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3722
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.48
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97176
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'light colourless'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.236
_refine_diff_density_min         -0.218
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         3722
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.959
_refine_ls_R_factor_all          0.0934
_refine_ls_R_factor_gt           0.0573
_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^)+(0.0499P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1090
_refine_ls_wR_factor_ref         0.1175
_reflns_number_gt                2532
_reflns_number_total             3722
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2018-482-275.cif
_cod_data_source_block           shi_3740_beda_twin1_hklf4
_cod_database_code               1563937
_chemical_oxdiff_formula         C20H20O4Na1
_chemical_oxdiff_usercomment     ICDB_45
_diffrn_oxdiff_twin_integration_method simultaneous
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6226(11)
 0.3774(11)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C3(H3), C7(H7), C12(H12), C9(H9), C14(H14), C16(H16), C4(H4),
 C13(H13), C15(H15), C10(H10)
3.b Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;