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_1563935
_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         'C44 H32 N4 O8 Zn2'
_chemical_formula_sum            'C44 H32 N4 O8 Zn2'
_chemical_formula_weight         875.48
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 97.819(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.7083(4)
_cell_length_b                   13.3839(6)
_cell_length_c                   13.3399(5)
_cell_measurement_reflns_used    5955
_cell_measurement_temperature    200.05(10)
_cell_measurement_theta_max      27.2040
_cell_measurement_theta_min      1.5710
_cell_volume                     1894.08(13)
_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      200.05(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
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -47.00  38.00   1.00   25.00    --  -23.85  77.00  30.00   85
  2  \w     66.00  94.00   1.00   25.00    --   26.04  77.00  90.00   28
  3  \w      2.00  94.00   1.00   25.00    --   26.04  77.00-120.00   92
  4  \w    -50.00 -11.00   1.00   25.00    --  -23.85  77.00 150.00   39
  5  \w    -96.00 -65.00   1.00   25.00    --  -23.85 178.00 120.00   31
  6  \w    -61.00 -35.00   1.00   25.00    --  -23.85-178.00   0.00   26
  7  \w    -91.00 -65.00   1.00   25.00    --  -23.85 -77.00 -30.00   26
  8  \w     35.00  76.00   1.00   25.00    --   26.04 178.00-120.00   41
  9  \w     13.00  86.00   1.00   25.00    --   26.04  57.00   0.00   73
 10  \w     21.00  47.00   1.00   25.00    --   26.04  77.00 150.00   26
;
_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      -0.0016650000
_diffrn_orient_matrix_UB_12      -0.0513597000
_diffrn_orient_matrix_UB_13      0.0128432000
_diffrn_orient_matrix_UB_21      -0.0519415000
_diffrn_orient_matrix_UB_22      -0.0071620000
_diffrn_orient_matrix_UB_23      -0.0383446000
_diffrn_orient_matrix_UB_31      0.0420979000
_diffrn_orient_matrix_UB_32      -0.0109253000
_diffrn_orient_matrix_UB_33      -0.0352593000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_unetI/netI     0.0511
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14908
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.92
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.329
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84734
_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    1.535
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.392
_refine_diff_density_min         -0.205
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.012(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     529
_refine_ls_number_reflns         6698
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0349
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0307P)^2^+0.0656P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0695
_refine_ls_wR_factor_ref         0.0718
_reflns_number_gt                6171
_reflns_number_total             6698
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2018-482-275.cif
_cod_data_source_block           shi_3674_dabe
_cod_database_code               1563935
_chemical_oxdiff_formula         C20H20N6O4Zn1
_chemical_oxdiff_usercomment     ICDB_32c
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O2X-C1 \\sim O2-C1
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O2) \\sim Ueq, Uanis(O2X) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O2X) = Uanis(O2)
4. Others
 Sof(O2)=1-FVAR(1)
 Sof(O2X)=FVAR(1)
5.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), C16(H16), C17(H17), C18(H18), C19(H19), C23(H23), C24(H24), C26(H26),
  C27(H27), C29(H29), C30(H30), C32(H32), C33(H33), C34(H34), C36(H36),
 C37(H37), C38(H38), C39(H39)
5.b Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C44(H44A,H44B,H44C)
;