18-Crown-6 Coordinated Metal Halides with Bright Luminescence and Nonlinear Optical Effects.
Merzlyakova, Elena; Wolf, Silke; Lebedkin, Sergei; Bayarjargal, Lkhamsuren; Neumeier, B. Lilli; Bartenbach, Daniel; Holzer, Christof; Klopper, Wim; Winkler, Bjoern; Kappes, Manfred; Feldmann, Claus; Journal of the American Chemical Society 143 (2021) 798–804; doi:10.1021/jacs.0c09454

data_4135584
_publ_contact_author
;
      Prof. Dr. Clas Feldmann
      Karlsruhe Institute of Technology (KIT), CS
      Institut fuer Anorganische Chemie (AOC)
      Engesserstr. 15, Geb. 30.45
      76131 Karlsruhe 
      Deutschland
;
_publ_section_title
;
 18-Crown-6 Coordinated Metal Halides with Bright Luminescence and
 Nonlinear Optical Effects.
;
_journal_issue                   2
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              798
_journal_page_last               804
_journal_paper_doi               10.1021/jacs.0c09454
_journal_volume                  143
_journal_year                    2021
_chemical_formula_moiety         'C12 H24 Br2 O6 Zn1'
_chemical_formula_sum            'C12 H24 Br2 O6 Zn'
_chemical_formula_weight         489.50
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_Hall           'R 3'
_space_group_name_H-M_alt        'R 3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-10-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   11.5448(16)
_cell_length_b                   11.5448(16)
_cell_length_c                   11.934(2)
_cell_measurement_reflns_used    5551
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.6
_cell_measurement_theta_min      2.6
_cell_volume                     1377.5(4)
_computing_cell_refinement       'CELL, SELECT (STOE)'
_computing_data_collection       'EXPOSE (STOE)'
_computing_data_reduction        'INTEGRATE (STOE)'
_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_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'image plate'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_unetI/netI     0.0465
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4172
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.983
_diffrn_reflns_theta_min         2.658
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    5.708
_exptl_absorpt_correction_T_max  0.4449
_exptl_absorpt_correction_T_min  0.3832
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
'(X-RED, Data Reduction Program, Version 1.61.1, Stoe & Cie GmbH, Darmstadt 2014.; X-SHAPE, Crystal Optimisation for Numerical Absorption Correction, Version 2.17, Stoe & Cie GmbH, Darmstadt 2014.)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.770
_exptl_crystal_description       cube
_exptl_crystal_F_000             732
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.055
_exptl_crystal_size_min          0.035
_refine_diff_density_max         0.248
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.54(7)
_refine_ls_extinction_coef       0.0005(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     72
_refine_ls_number_reflns         1610
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0308
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0183P)^2^+0.9586P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0468
_refine_ls_wR_factor_ref         0.0527
_reflns_Friedel_coverage         0.988
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.972
_reflns_number_gt                1224
_reflns_number_total             1610
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c09454_si_003.cif
_cod_data_source_block           ZnBr2(18-crown-6)
_cod_original_cell_volume        1377.5(5)
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               4135584
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.46(7)
 0.54(7)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
3. Others
 Fixed Sof: Zn1(0.33333)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B)
;
_olex2_submission_special_instructions 'No special instructions were received'