Two low-dimensional metal halides: ionothermal synthesis, photoluminescence, and nonlinear optical properties
Deng, Yuandan; Dong, Xuehua; Yang, Meng; Zeng, Hongmei; Zou, Guohong; Lin, Zhien; Dalton Transactions  (2019) –; doi:10.1039/C9DT04102H

data_7701864
_publ_section_title
;
 Two low-dimensional metal halides: ionothermal synthesis,
 photoluminescence, and nonlinear optical properties
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT04102H
_journal_year                    2019
_chemical_formula_moiety         'Cl4 Mn, 2(C7 H13 N2)'
_chemical_formula_sum            'C14 H26 Cl4 Mn N4'
_chemical_formula_weight         447.13
_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
_audit_creation_date             2019-08-26
_audit_creation_method
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Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-10-19 deposited with the CCDC.	2019-11-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.249(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.3865(5)
_cell_length_b                   9.30665(16)
_cell_length_c                   15.4932(4)
_cell_measurement_reflns_used    5464
_cell_measurement_temperature    293.11(10)
_cell_measurement_theta_max      72.5440
_cell_measurement_theta_min      4.7730
_cell_volume                     2154.30(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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_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      air
_diffrn_ambient_temperature      293.11(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9595
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega    1.00   75.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -99.0000  -30.0000 74

  2 omega    1.00   75.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -99.0000 -150.0000 74

  3 omega   10.00  104.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       36.5421   77.0000 -180.0000 94

  4 omega  -35.00   66.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -19.0000    0.0000 101

  5 omega   20.00  104.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       36.5421   57.0000  -30.0000 84

  6 omega   23.00   90.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       36.5421 -125.0000  120.0000 67

  7 omega   38.00   91.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -90.0000 53

  8 omega   38.00   91.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   60.0000 53

  9 omega   38.00   91.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -150.0000 53

 10 omega   90.00  175.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000 -180.0000 85

 11 omega   39.00  109.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000  120.0000 70

 12 omega   90.00  175.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000   90.0000 85

 13 omega   40.00   98.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000 -180.0000 58

 14 omega   38.00   91.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -60.0000 53

 15 omega   40.00   98.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000    0.0000 58

 16 omega   70.00  178.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000   60.0000 108

 17 omega   10.00   91.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       36.5421   77.0000   60.0000 81
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Gemini, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0924072000
_diffrn_orient_matrix_UB_12      -0.0072544000
_diffrn_orient_matrix_UB_13      -0.0039216000
_diffrn_orient_matrix_UB_21      -0.0329703000
_diffrn_orient_matrix_UB_22      -0.1246306000
_diffrn_orient_matrix_UB_23      -0.0714348000
_diffrn_orient_matrix_UB_31      -0.0318120000
_diffrn_orient_matrix_UB_32      0.1086647000
_diffrn_orient_matrix_UB_33      -0.0822383000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11592
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.079
_diffrn_reflns_theta_max         67.079
_diffrn_reflns_theta_min         5.601
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.567
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27262
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_description       plate
_exptl_crystal_F_000             924
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.650
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.080
_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     214
_refine_ls_number_reflns         3845
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0531
_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^)+(0.1039P)^2^+0.4750P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1435
_refine_ls_wR_factor_ref         0.1535
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3291
_reflns_number_total             3845
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04102h2.cif
_cod_data_source_block           yd1-40-4
_cod_original_cell_volume        2154.29(10)
_cod_database_code               7701864
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.393
_shelx_estimated_absorpt_t_min   0.130
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C13(H13A,H13B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C11(H11), C12(H12)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,
 H10B,H10C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              98172
_olex2_date_sample_data_collection 2019-03-08
_olex2_submission_special_instructions 'No special instructions were received'