#------------------------------------------------------------------------------
#$Date: 2019-11-03 14:58:29 +0200 (Sun, 03 Nov 2019) $
#$Revision: 221694 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/86/4128613.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_4128613
loop_
_publ_author_name
'Peng, Yu'
'Li, Lina'
'Ji, Chengmin'
'Wu, Zhenyue'
'Wang, Sasa'
'Liu, Xitao'
'Yao, Yunpeng'
'Luo, Junhua'
_publ_section_title
;
 Tailored Synthesis of an Unprecedented Pb-Mn Heterometallic Halide Hybrid
 with Enhanced Emission.
;
_journal_issue                   31
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12197
_journal_page_last               12201
_journal_paper_doi               10.1021/jacs.9b04829
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         '0.5(Cl28 Pb10), 2(C5 H14 N2)'
_chemical_formula_sum            'C10 H28 Cl14 N4 Pb5'
_chemical_formula_weight         1736.61
_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_Hall           'C 2c 2'
_space_group_name_H-M_alt        'C 2 2 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-04-22
_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                90
_cell_formula_units_Z            4
_cell_length_a                   10.7997(4)
_cell_length_b                   18.2694(6)
_cell_length_c                   16.8270(6)
_cell_measurement_reflns_used    3721
_cell_measurement_temperature    285(2)
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      2.50
_cell_volume                     3320.0(2)
_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-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      285.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0647
_diffrn_reflns_av_unetI/netI     0.0707
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9839
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         2.191
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    26.410
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.474
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             3056
_refine_diff_density_max         1.214
_refine_diff_density_min         -1.953
_refine_diff_density_rms         0.361
_refine_ls_abs_structure_details
;
 Flack x determined using 837 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.03(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         2931
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0451
_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)+(0.0420P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0961
_refine_ls_wR_factor_ref         0.1039
_reflns_Friedel_coverage         0.775
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                2382
_reflns_number_total             2931
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja9b04829_si_002.cif
_cod_data_source_block           1
_cod_database_code               4128613
_shelx_shelxl_version_number     2017/1
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All N(H,H,H) groups
2. Rigid bond restraints
 C1, C2, C3, C4, C5, N1, N2
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim N1 \\sim N2: within 2A with sigma
of 0.005 and sigma for terminal atoms of 0.01
4.a Ternary CH refined with riding coordinates:
 C1(H)
4.b Secondary CH2 refined with riding coordinates:
 N2(HA,HB), C4(HC,HD), C3(HE,HF), C5(HJ,HK), C2(HL,HM)
4.c Idealised Me refined as rotating group:
 N1(HG,HH,HI)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x, -y, -z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z+1/2'
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
Pb3 Pb 0.000000 0.17332(6) 0.250000 0.0229(3) Uani 1 2 d S T P
Pb2 Pb 0.18896(8) 0.37411(4) 0.24805(13) 0.0239(3) Uani 1 1 d . . .
Pb1 Pb 0.49657(18) 0.46240(4) 0.37563(6) 0.0242(3) Uani 1 1 d . . .
Cl6 Cl -0.0029(12) 0.3006(3) 0.3501(3) 0.0233(12) Uani 1 1 d . . .
Cl7 Cl 0.000000 0.4824(4) 0.250000 0.0248(17) Uani 1 2 d S T P
Cl1 Cl 0.6598(4) 0.5249(2) 0.2491(8) 0.0216(12) Uani 1 1 d . . .
Cl4 Cl 0.500000 0.3536(4) 0.250000 0.0286(19) Uani 1 2 d S T P
Cl8 Cl 0.2563(5) 0.2105(3) 0.2482(10) 0.0253(13) Uani 1 1 d . . .
Cl2 Cl 0.7475(8) 0.4259(7) 0.4097(7) 0.037(3) Uani 1 1 d . . .
Cl5 Cl 0.2359(8) 0.4217(6) 0.4191(6) 0.028(2) Uani 1 1 d . . .
Cl3 Cl 0.5066(13) 0.6071(3) 0.4270(4) 0.0416(17) Uani 1 1 d . . .
C1 C 0.048(2) 0.3627(13) 0.6125(18) 0.027(3) Uani 1 1 d . U .
H H 0.031632 0.354046 0.669086 0.032 Uiso 1 1 calc R . .
N2 N -0.0673(19) 0.2516(12) 0.5768(15) 0.030(3) Uani 1 1 d . U .
HA H -0.062028 0.209064 0.551338 0.036 Uiso 1 1 calc R . .
HB H -0.079879 0.242145 0.628084 0.036 Uiso 1 1 calc R . .
C4 C -0.175(3) 0.2939(14) 0.5450(18) 0.029(3) Uani 1 1 d . U .
HC H -0.167608 0.299681 0.487915 0.035 Uiso 1 1 calc R . .
HD H -0.251837 0.267773 0.555852 0.035 Uiso 1 1 calc R . .
C3 C -0.178(3) 0.3648(14) 0.583(2) 0.027(3) Uani 1 1 d . U .
HE H -0.193320 0.358292 0.639290 0.033 Uiso 1 1 calc R . .
HF H -0.246247 0.393039 0.561203 0.033 Uiso 1 1 calc R . .
N1 N 0.161(2) 0.3999(12) 0.6002(14) 0.027(4) Uani 1 1 d . U .
HG H 0.220170 0.378972 0.629250 0.041 Uiso 1 1 calc GR . .
HH H 0.152791 0.446496 0.614583 0.041 Uiso 1 1 calc GR . .
HI H 0.181469 0.397555 0.549026 0.041 Uiso 1 1 calc GR . .
C5 C 0.056(2) 0.2936(14) 0.5673(18) 0.027(3) Uani 1 1 d . U .
HJ H 0.124176 0.264164 0.587316 0.033 Uiso 1 1 calc R . .
HK H 0.071385 0.303946 0.511645 0.033 Uiso 1 1 calc R . .
C2 C -0.059(2) 0.4074(14) 0.5720(17) 0.027(3) Uani 1 1 d . U .
HL H -0.066200 0.455350 0.596454 0.032 Uiso 1 1 calc R . .
HM H -0.041688 0.413973 0.515917 0.032 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 0.0033 0.0016 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 '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
Cl6 Pb3 Cl6 71.8(2) . 4
Cl6 Pb3 Cl1 132.4(3) . 8_545
Cl6 Pb3 Cl1 133.8(3) 4 8_545
Cl6 Pb3 Cl1 133.8(3) . 5_445
Cl6 Pb3 Cl1 132.4(3) 4 5_445
Cl6 Pb3 Cl3 147.93(15) 4 5_445
Cl6 Pb3 Cl3 76.21(14) . 5_445
Cl1 Pb3 Cl1 64.95(17) 8_545 5_445
Cl1 Pb3 Cl3 72.0(3) 8_545 5_445
Cl1 Pb3 Cl3 71.0(3) 5_445 5_445
Cl8 Pb3 Cl6 77.9(4) . 4
Cl8 Pb3 Cl6 77.9(4) 4 .
Cl8 Pb3 Cl6 79.8(3) . .
Cl8 Pb3 Cl6 79.8(3) 4 4
Cl8 Pb3 Cl1 71.33(13) 4 8_545
Cl8 Pb3 Cl1 136.28(13) . 8_545
Cl8 Pb3 Cl1 136.28(13) 4 5_445
Cl8 Pb3 Cl1 71.33(13) . 5_445
Cl8 Pb3 Cl8 152.4(2) . 4
Cl8 Pb3 Cl3 94.5(4) . 5_445
Cl8 Pb3 Cl3 95.8(4) 4 5_445
Cl6 Pb2 Cl6 69.16(17) 4 .
Cl6 Pb2 Cl1 136.6(2) . 4_655
Cl6 Pb2 Cl1 138.9(2) 4 4_655
Cl6 Pb2 Cl8 73.6(3) 4 .
Cl6 Pb2 Cl8 74.3(2) . .
Cl6 Pb2 Cl5 141.0(2) 4 .
Cl6 Pb2 Cl5 72.7(2) . .
Cl7 Pb2 Cl6 80.4(2) . 4
Cl7 Pb2 Cl6 79.00(19) . .
Cl7 Pb2 Cl1 76.55(13) . 4_655
Cl7 Pb2 Cl8 147.78(14) . .
Cl7 Pb2 Cl2 87.3(2) . 4_655
Cl7 Pb2 Cl5 84.83(19) . .
Cl8 Pb2 Cl1 135.65(13) . 4_655
Cl2 Pb2 Cl6 146.2(2) 4_655 .
Cl2 Pb2 Cl6 78.2(2) 4_655 4
Cl2 Pb2 Cl1 67.2(3) 4_655 4_655
Cl2 Pb2 Cl8 105.2(4) 4_655 .
Cl2 Pb2 Cl5 137.0(2) 4_655 .
Cl5 Pb2 Cl1 69.9(3) . 4_655
Cl5 Pb2 Cl8 103.7(4) . .
Cl1 Pb1 Cl1 71.40(16) 4_655 .
Cl1 Pb1 Cl5 145.2(3) . .
Cl1 Pb1 Cl5 74.3(2) 4_655 .
Cl4 Pb1 Cl1 74.63(19) . .
Cl4 Pb1 Cl1 75.63(18) . 4_655
Cl4 Pb1 Cl5 91.2(2) . .
Cl2 Pb1 Cl1 70.8(3) . .
Cl2 Pb1 Cl1 141.7(3) . 4_655
Cl2 Pb1 Cl4 88.5(3) . .
Cl2 Pb1 Cl5 141.73(19) . .
Cl3 Pb1 Cl1 82.8(2) . 4_655
Cl3 Pb1 Cl1 80.5(3) . .
Cl3 Pb1 Cl4 151.18(18) . .
Cl3 Pb1 Cl2 97.0(4) . .
Cl3 Pb1 Cl5 101.3(3) . .
Pb3 Cl6 Pb2 91.1(2) . .
Pb3 Cl6 Pb2 92.8(2) . 4
Pb2 Cl6 Pb2 86.93(13) 4 .
Pb2 Cl7 Pb2 91.80(19) . 4
Pb1 Cl1 Pb1 91.23(13) 4_655 .
Pb1 Cl4 Pb1 93.56(19) . 4_655
Pb3 Cl8 Pb2 90.12(14) . .
Pb1 Cl2 Pb2 96.7(3) . 4_655
Pb1 Cl5 Pb2 89.8(3) . .
Pb1 Cl3 Pb3 93.93(18) . 8
N1 C1 H 112.0 . .
N1 C1 C5 106(2) . .
N1 C1 C2 109(2) . .
C5 C1 H 112.0 . .
C5 C1 C2 105(2) . .
C2 C1 H 112.0 . .
HA N2 HB 107.9 . .
C4 N2 HA 109.1 . .
C4 N2 HB 109.1 . .
C4 N2 C5 112.3(18) . .
C5 N2 HA 109.1 . .
C5 N2 HB 109.1 . .
N2 C4 HC 110.0 . .
N2 C4 HD 110.0 . .
HC C4 HD 108.3 . .
C3 C4 N2 109(2) . .
C3 C4 HC 110.0 . .
C3 C4 HD 110.0 . .
C4 C3 HE 109.0 . .
C4 C3 HF 109.0 . .
C4 C3 C2 113(2) . .
HE C3 HF 107.8 . .
C2 C3 HE 109.0 . .
C2 C3 HF 109.0 . .
C1 N1 HG 109.5 . .
C1 N1 HH 109.5 . .
C1 N1 HI 109.5 . .
HG N1 HH 109.5 . .
HG N1 HI 109.5 . .
HH N1 HI 109.5 . .
C1 C5 N2 109(2) . .
C1 C5 HJ 110.0 . .
C1 C5 HK 110.0 . .
N2 C5 HJ 110.0 . .
N2 C5 HK 110.0 . .
HJ C5 HK 108.4 . .
C1 C2 HL 110.2 . .
C1 C2 HM 110.2 . .
C3 C2 C1 108(2) . .
C3 C2 HL 110.2 . .
C3 C2 HM 110.2 . .
HL C2 HM 108.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb3 Cl6 2.872(5) .
Pb3 Cl6 2.872(5) 4
Pb3 Cl1 3.215(5) 8_545
Pb3 Cl1 3.215(5) 5_445
Pb3 Cl8 2.851(5) .
Pb3 Cl8 2.851(5) 4
Pb3 Cl3 3.215(7) 5_445
Pb2 Cl6 3.007(10) .
Pb2 Cl6 2.927(10) 4
Pb2 Cl7 2.842(5) .
Pb2 Cl1 3.202(5) 4_655
Pb2 Cl8 3.076(5) .
Pb2 Cl2 2.900(12) 4_655
Pb2 Cl5 3.050(11) .
Pb1 Cl1 2.926(11) 4_655
Pb1 Cl1 2.991(10) .
Pb1 Cl4 2.901(5) .
Pb1 Cl2 2.849(9) .
Pb1 Cl5 3.002(9) .
Pb1 Cl3 2.784(6) .
C1 H 0.9800 .
C1 N1 1.41(3) .
C1 C5 1.48(4) .
C1 C2 1.57(3) .
N2 HA 0.8900 .
N2 HB 0.8900 .
N2 C4 1.50(3) .
N2 C5 1.55(3) .
C4 HC 0.9700 .
C4 HD 0.9700 .
C4 C3 1.44(4) .
C3 HE 0.9700 .
C3 HF 0.9700 .
C3 C2 1.51(4) .
N1 HG 0.8900 .
N1 HH 0.8900 .
N1 HI 0.8900 .
C5 HJ 0.9700 .
C5 HK 0.9700 .
C2 HL 0.9700 .
C2 HM 0.9700 .
