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_4135582
_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 Cl5 Mn2 O6, C12 H24 Cl Mn O6'
_chemical_formula_sum            'C24 H48 Cl6 Mn3 O12'
_chemical_formula_weight         906.14
_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
_audit_creation_date             2019-12-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 124.63(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.670(3)
_cell_length_b                   10.642(2)
_cell_length_c                   25.798(8)
_cell_measurement_reflns_used    17550
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      29.3
_cell_measurement_theta_min      1.5
_cell_volume                     3765.8(18)
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.989
_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  0.0243
_diffrn_reflns_av_unetI/netI     0.0548
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            35253
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.272
_diffrn_reflns_theta_min         2.141
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.468
_exptl_absorpt_correction_T_max  0.887
_exptl_absorpt_correction_T_min  0.773
_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    1.598
_exptl_crystal_description       block
_exptl_crystal_F_000             1860
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.037
_refine_diff_density_min         -0.676
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.826
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         10173
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      0.840
_refine_ls_R_factor_all          0.1012
_refine_ls_R_factor_gt           0.0556
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1004P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1551
_refine_ls_wR_factor_ref         0.1683
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4506
_reflns_number_total             10173
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c09454_si_005.cif
_cod_data_source_block           mn3cl6(18c6)2
_cod_original_cell_volume        3765.8(17)
_cod_database_code               4135582
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Restrained distances
 C20-O11 = C21-O11 = C22-O12 = C23-O12
 1.45 with sigma of 0.02
 C21-C22 = C23-C24
 1.54 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O11) \\sim Ueq, Uanis(O12) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(C20) = Uanis(C19)
Uanis(C21) = Uanis(C22)
4.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C16(H16A,H16B), C24(H24A,H24B), C18(H18A,H18B), C20(H20B,
 H20A), C23(H23A,H23B), C19(H19A,H19B), C21(H21A,H21B), C14(H14A,H14B),
 C17(H17A,H17B), C13(H13A,H13B), C22(H22A,H22B), C7(H7A,H7B), C9(H9A,H9B),
 C10(H10A,H10B), C11(H11A,H11B), C1(H1A,H1B), C6(H6A,H6B), C4(H4A,H4B),
 C12(H12A,H12B), C8(H8A,H8B), C2(H2A,H2B), C5(H5A,H5B), C3(H3A,H3B)
;
_shelx_res_checksum              1090
_shelx_hkl_checksum              12641
_olex2_submission_special_instructions 'No special instructions were received'