#------------------------------------------------------------------------------
#$Date: 2021-11-04 01:58:51 +0200 (Thu, 04 Nov 2021) $
#$Revision: 270276 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/86/7708693.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7708693
loop_
_publ_author_name
'Zhang, Yue'
'Chen, Dian'
'Jin, Kai-Hang'
'Zang, Shuang-Quan'
'Wang, Qing-Lun'
_publ_section_title
;
 Room-temperature phosphorescence of manganese-based metal halides
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03206B
_journal_year                    2021
_chemical_formula_moiety         'Cl6 Mn, 2(C8 H14 N2)'
_chemical_formula_sum            'C16 H28 Cl6 Mn N4'
_chemical_formula_weight         544.06
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-02-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-09-17 deposited with the CCDC.	2021-11-01 downloaded from the CCDC.
;
_cell_angle_alpha                101.991(3)
_cell_angle_beta                 99.889(3)
_cell_angle_gamma                112.943(3)
_cell_formula_units_Z            1
_cell_length_a                   7.5206(3)
_cell_length_b                   8.4873(3)
_cell_length_c                   10.5291(3)
_cell_measurement_reflns_used    3780
_cell_measurement_temperature    296.6(6)
_cell_measurement_theta_max      72.7890
_cell_measurement_theta_min      5.9230
_cell_volume                     581.08(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (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      air
_diffrn_ambient_temperature      296.6(6)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -57.00   0.00   0.50    0.50    --    0.00 -38.00  90.00  114
  2  ω    -56.00  12.00   0.50    0.50    --    0.00 -37.00-176.00  136
  3  ω    -13.00  29.00   0.50    0.50    --    0.00 -38.00 -60.00   84
  4  ω    -87.00 -37.00   0.50    0.50    --    0.00 -38.00 -60.00  100
  5  ω      8.00 135.00   0.50    0.50    --   97.60 -82.00   0.00  254
  6  ω      9.00  61.00   0.50    0.50    --   97.60 -61.00-150.00  104
  7  ω    133.00 159.00   0.50    0.50    --   97.60  77.00  60.00   52
  8  ω      8.00 127.00   0.50    0.50    --   97.60 -82.00-150.00  238
  9  ω     92.00 118.00   0.50    0.50    --   97.60 -82.00 120.00   52
 10  ω     64.00 186.00   0.50    0.50    --   97.60  30.00  90.00  244
 11  ω    101.00 130.00   0.50    0.50    --   97.60 -30.00 120.00   58
 12  ω     86.00 123.00   0.50    0.50    --   97.60  45.00 120.00   74
 13  ω     21.00  47.00   0.50    0.50    --   97.60 -30.00 120.00   52
 14  ω     69.00 128.00   0.50    0.50    --   97.60 -61.00-150.00  118
 15  ω     33.00  58.00   0.50    0.50    --   97.60 -82.00 120.00   50
 16  ω    128.00 161.00   0.50    0.50    --   97.60  45.00 120.00   66
 17  ω     71.00 105.00   0.50    0.50    --   97.60  77.00  60.00   68
 18  ω     89.00 114.00   0.50    0.50    --   97.60 -82.00 -90.00   50
 19  ω     65.00 135.00   0.50    0.50    --   97.60 -82.00  60.00  140
 20  ω     98.00 130.00   0.50    0.50    --   97.60  45.00-180.00   64
 21  ω     89.00 115.00   0.50    0.50    --   97.60 -82.00  90.00   52
 22  ω     81.00 183.00   0.50    0.50    --   97.60  61.00 150.00  204
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0169878000
_diffrn_orient_matrix_UB_12      -0.1730990000
_diffrn_orient_matrix_UB_13      0.0074552000
_diffrn_orient_matrix_UB_21      0.2272625000
_diffrn_orient_matrix_UB_22      0.1104245000
_diffrn_orient_matrix_UB_23      0.0694795000
_diffrn_orient_matrix_UB_31      -0.0415583000
_diffrn_orient_matrix_UB_32      0.0242963000
_diffrn_orient_matrix_UB_33      0.1391190000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5478
_diffrn_reflns_av_R_equivalents  0.0252
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4761
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        68.230
_diffrn_reflns_theta_max         73.781
_diffrn_reflns_theta_min         4.490
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.160
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.35881
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_description       block
_exptl_crystal_F_000             279
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.334
_refine_diff_density_min         -0.681
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     126
_refine_ls_number_reflns         2227
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0376
_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/[σ²(Fo²)+(0.0690P)²+0.0868P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0973
_refine_ls_wR_factor_ref         0.0981
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2139
_reflns_number_total             2227
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt03206b2.cif
_cod_data_source_block           2
_cod_original_cell_volume        581.09(3)
_cod_database_code               7708693
_shelx_shelxl_version_number     2016/4
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_reflns_odcompleteness_completeness 98.22
_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, All N(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1D,H1E), C8(H8A,H8B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7)
2.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N2(H2A,H2B,H2C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.013
_oxdiff_exptl_absorpt_empirical_full_min 0.643
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.000000 0.500000 0.000000 0.02126(15) Uani 1 2 d S T P . .
Cl1 Cl 0.14198(7) 0.26762(6) -0.00536(5) 0.02363(15) Uani 1 1 d . . . . .
Cl2 Cl 0.01214(7) 0.52340(7) 0.24358(5) 0.02661(16) Uani 1 1 d . . . . .
Cl3 Cl -0.37260(7) 0.23826(7) -0.06937(6) 0.02908(16) Uani 1 1 d . . . . .
N1 N 0.5811(3) 0.5298(2) 0.18660(18) 0.0257(4) Uani 1 1 d . . . . .
H1A H 0.518004 0.428913 0.117647 0.031 Uiso 1 1 calc GR . . . .
H1B H 0.713410 0.570909 0.200135 0.031 Uiso 1 1 calc GR . . . .
H1C H 0.543435 0.611554 0.167770 0.031 Uiso 1 1 calc GR . . . .
N2 N 1.1698(3) 0.9104(2) 0.83594(19) 0.0275(4) Uani 1 1 d . . . . .
H2A H 1.099317 0.799823 0.838726 0.033 Uiso 1 1 calc GR . . . .
H2B H 1.124336 0.983506 0.876826 0.033 Uiso 1 1 calc GR . . . .
H2C H 1.298999 0.948631 0.878021 0.033 Uiso 1 1 calc GR . . . .
C1 C 0.5284(4) 0.4931(3) 0.3106(2) 0.0344(5) Uani 1 1 d . . . . .
H1D H 0.563041 0.399367 0.328132 0.041 Uiso 1 1 calc R . . . .
H1E H 0.384471 0.450284 0.296102 0.041 Uiso 1 1 calc R . . . .
C2 C 0.6372(3) 0.6585(3) 0.4320(2) 0.0257(4) Uani 1 1 d . . . . .
C3 C 0.5421(4) 0.7619(3) 0.4731(2) 0.0319(5) Uani 1 1 d . . . . .
H3 H 0.411391 0.730776 0.424801 0.038 Uiso 1 1 calc R . . . .
C4 C 0.6415(4) 0.9126(3) 0.5869(3) 0.0359(5) Uani 1 1 d . . . . .
H4 H 0.576380 0.980927 0.615123 0.043 Uiso 1 1 calc R . . . .
C5 C 0.8361(4) 0.9606(3) 0.6577(2) 0.0320(5) Uani 1 1 d . . . . .
H5 H 0.902655 1.062862 0.732390 0.038 Uiso 1 1 calc R . . . .
C6 C 0.9337(3) 0.8577(3) 0.6183(2) 0.0257(4) Uani 1 1 d . . . . .
C7 C 0.8325(3) 0.7055(3) 0.5055(2) 0.0262(4) Uani 1 1 d . . . . .
H7 H 0.895938 0.634737 0.479164 0.031 Uiso 1 1 calc R . . . .
C8 C 1.1479(3) 0.9093(4) 0.6933(2) 0.0351(5) Uani 1 1 d . . . . .
H8A H 1.191679 0.825223 0.648035 0.042 Uiso 1 1 calc R . . . .
H8B H 1.234288 1.027753 0.690750 0.042 Uiso 1 1 calc R . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0193 0.0097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3694 0.7045 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn -0.5661 2.8539 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0328 0.0186 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1 Mn1 Cl1 180.0 2_565 . ?
Cl1 Mn1 Cl3 89.852(15) . 2_565 ?
Cl1 Mn1 Cl3 89.851(15) 2_565 . ?
Cl1 Mn1 Cl3 90.149(15) 2_565 2_565 ?
Cl1 Mn1 Cl3 90.149(15) . . ?
Cl2 Mn1 Cl1 88.831(16) . . ?
Cl2 Mn1 Cl1 91.169(16) 2_565 . ?
Cl2 Mn1 Cl1 91.168(16) . 2_565 ?
Cl2 Mn1 Cl1 88.832(16) 2_565 2_565 ?
Cl2 Mn1 Cl2 180.0 2_565 . ?
Cl2 Mn1 Cl3 91.587(17) . 2_565 ?
Cl2 Mn1 Cl3 88.413(17) 2_565 2_565 ?
Cl2 Mn1 Cl3 91.586(17) 2_565 . ?
Cl2 Mn1 Cl3 88.414(17) . . ?
Cl3 Mn1 Cl3 180.0 2_565 . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
H2A N2 H2B 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
C8 N2 H2A 109.5 . . ?
C8 N2 H2B 109.5 . . ?
C8 N2 H2C 109.5 . . ?
N1 C1 H1D 109.3 . . ?
N1 C1 H1E 109.3 . . ?
N1 C1 C2 111.72(17) . . ?
H1D C1 H1E 107.9 . . ?
C2 C1 H1D 109.3 . . ?
C2 C1 H1E 109.3 . . ?
C3 C2 C1 120.2(2) . . ?
C3 C2 C7 119.5(2) . . ?
C7 C2 C1 120.2(2) . . ?
C2 C3 H3 119.9 . . ?
C2 C3 C4 120.1(2) . . ?
C4 C3 H3 119.9 . . ?
C3 C4 H4 119.9 . . ?
C5 C4 C3 120.2(2) . . ?
C5 C4 H4 119.9 . . ?
C4 C5 H5 119.7 . . ?
C4 C5 C6 120.5(2) . . ?
C6 C5 H5 119.7 . . ?
C5 C6 C7 119.1(2) . . ?
C5 C6 C8 121.4(2) . . ?
C7 C6 C8 119.5(2) . . ?
C2 C7 C6 120.5(2) . . ?
C2 C7 H7 119.7 . . ?
C6 C7 H7 119.7 . . ?
N2 C8 C6 112.21(18) . . ?
N2 C8 H8A 109.2 . . ?
N2 C8 H8B 109.2 . . ?
C6 C8 H8A 109.2 . . ?
C6 C8 H8B 109.2 . . ?
H8A C8 H8B 107.9 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 Cl1 2.5787(4) . ?
Mn1 Cl1 2.5786(4) 2_565 ?
Mn1 Cl2 2.5138(5) . ?
Mn1 Cl2 2.5138(5) 2_565 ?
Mn1 Cl3 2.6627(5) 2_565 ?
Mn1 Cl3 2.6628(5) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C1 1.486(3) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 H2C 0.8900 . ?
N2 C8 1.480(3) . ?
C1 H1D 0.9700 . ?
C1 H1E 0.9700 . ?
C1 C2 1.508(3) . ?
C2 C3 1.381(3) . ?
C2 C7 1.393(3) . ?
C3 H3 0.9300 . ?
C3 C4 1.393(3) . ?
C4 H4 0.9300 . ?
C4 C5 1.377(3) . ?
C5 H5 0.9300 . ?
C5 C6 1.388(3) . ?
C6 C7 1.394(3) . ?
C6 C8 1.510(3) . ?
C7 H7 0.9300 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
