#------------------------------------------------------------------------------
#$Date: 2021-09-06 13:09:18 +0200 (lun 06 de sep de 2021) $
#$Revision: 268754 $
#$URL: svn://www.crystallography.net/cod/cif/7/70/79/7707925.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_7707925
loop_
_publ_author_name
'Zhang, Lu'
'Ma, Wen'
'Sun, Chen'
'Fang, Lei'
'Song, Xueling'
'Fei, Honghan'
_publ_section_title
;
 Precise incorporation of transition metals into organolead oxyhalide
 crystalline materials for photocatalysis.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11360
_journal_page_last               11364
_journal_paper_doi               10.1039/d1dt01621k
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         '0.5(C12 H24 Br18 Mn2 O16 Pb16)'
_chemical_formula_sum            'C6 H12 Br9 Mn O8 Pb8'
_chemical_formula_weight         2643.81
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-10-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-05-10 deposited with the CCDC.	2021-07-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.563(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.6712(6)
_cell_length_b                   9.1623(4)
_cell_length_c                   18.0456(10)
_cell_measurement_reflns_used    2890
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      26.35
_cell_measurement_theta_min      3.06
_cell_volume                     1597.43(15)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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  0.0505
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16996
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.385
_diffrn_reflns_theta_min         3.064
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    53.656
_exptl_absorpt_correction_T_max  0.0123
_exptl_absorpt_correction_T_min  0.0012
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1514 before and 0.0813 after correction.
The Ratio of minimum to maximum transmission is 0.0976.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    5.497
_exptl_crystal_description       block
_exptl_crystal_F_000             2216
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_refine_diff_density_max         4.171
_refine_diff_density_min         -3.652
_refine_diff_density_rms         0.597
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         3275
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0581
_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/[σ²(Fo²)+(0.1192P)²+5.6327P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1559
_refine_ls_wR_factor_ref         0.1588
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2989
_reflns_number_total             3275
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt01621k2.cif
_cod_data_source_block           mo_190923a_a
_cod_depositor_comments          'Adding full bibliography for 7707925.cif.'
_cod_database_code               7707925
_shelx_shelxl_version_number     2014/7
_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.
;
_shelx_estimated_absorpt_t_max   0.050
_shelx_estimated_absorpt_t_min   0.030
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C0AA(H0AA,H0AB)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.18595(6) 0.54975(6) 0.58628(3) 0.0394(2) Uani 1 1 d . . . . .
O1 O 0.6593(10) 0.8406(10) 0.6883(6) 0.035(2) Uani 1 1 d . . . . .
Br1 Br 0.14268(17) 0.85950(16) 0.54345(9) 0.0454(4) Uani 1 1 d . . . . .
Mn1 Mn 0.7500 1.0209(3) 0.7500 0.0317(6) Uani 1 2 d S T P . .
C1 C 0.5362(16) 1.1407(18) 0.8463(9) 0.042(3) Uani 1 1 d . . . . .
H1A H 0.5156 1.2044 0.8872 0.050 Uiso 1 1 calc R . . . .
H1B H 0.4729 1.0586 0.8464 0.050 Uiso 1 1 calc R . . . .
Pb2 Pb 0.43296(5) 0.92444(6) 0.65622(3) 0.0380(2) Uani 1 1 d . . . . .
C2 C 0.6807(17) 0.7069(16) 0.7321(9) 0.041(3) Uani 1 1 d . . . . .
H2A H 0.6119 0.7010 0.7695 0.049 Uiso 1 1 calc R . . . .
H2B H 0.6698 0.6223 0.7000 0.049 Uiso 1 1 calc R . . . .
Br2 Br 0.47391(15) 0.64210(16) 0.56737(8) 0.0414(3) Uani 1 1 d . . . . .
C0AA C 0.9824(16) 1.2236(16) 0.7267(8) 0.038(3) Uani 1 1 d . . . . .
H0AA H 1.0794 1.2472 0.7361 0.046 Uiso 1 1 calc R . . . .
H0AB H 0.9305 1.3142 0.7238 0.046 Uiso 1 1 calc R . . . .
Pb3 Pb 0.77209(6) 0.88069(6) 0.56808(3) 0.0412(2) Uani 1 1 d . . . . .
O3 O 0.5691(10) 1.0131(10) 0.5643(5) 0.0340(19) Uani 1 1 d . . . . .
Br3 Br 0.2500 0.6413(4) 0.7500 0.0737(8) Uani 1 2 d S T P . .
Pb4 Pb 0.62434(6) 1.24643(6) 0.59980(3) 0.0393(2) Uani 1 1 d . . . . .
O4 O 0.6784(10) 1.0886(10) 0.8551(6) 0.035(2) Uani 1 1 d . . . . .
Br4 Br 0.30029(16) 0.24161(15) 0.60195(9) 0.0423(4) Uani 1 1 d . . . . .
Br5 Br 0.13522(16) 0.48277(17) 0.42231(9) 0.0447(4) Uani 1 1 d . . . . .
O5 O 0.9343(11) 1.1355(11) 0.7860(5) 0.037(2) Uani 1 1 d . . . . .
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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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
_geom_angle_publ_flag
Br1 Pb1 Br3 90.53(7) . . ?
Br1 Pb1 Br4 163.56(5) . . ?
Br1 Pb1 Br5 85.69(5) . . ?
Br1 Pb1 Br5 87.13(5) . 3_566 ?
Br2 Pb1 Br1 79.51(5) . . ?
Br2 Pb1 Br3 83.30(4) . . ?
Br2 Pb1 Br4 86.31(4) . . ?
Br2 Pb1 Br5 93.29(4) . . ?
Br2 Pb1 Br5 165.24(5) . 3_566 ?
Br3 Pb1 Br5 103.24(4) . 3_566 ?
Br4 Pb1 Br3 96.09(7) . . ?
Br4 Pb1 Br5 105.86(4) . 3_566 ?
Br5 Pb1 Br3 175.32(6) . . ?
Br5 Pb1 Br4 86.86(5) . . ?
Br5 Pb1 Br5 79.35(5) . 3_566 ?
Mn1 O1 Pb2 103.2(4) . . ?
Mn1 O1 Pb3 98.8(4) . . ?
Pb2 O1 Pb3 100.0(3) . . ?
C2 O1 Mn1 108.5(8) . . ?
C2 O1 Pb2 120.6(8) . . ?
C2 O1 Pb3 122.3(9) . . ?
O1 Mn1 O1 80.0(5) . 2_656 ?
O4 Mn1 O1 84.5(4) 2_656 . ?
O4 Mn1 O1 122.6(4) . . ?
O4 Mn1 O1 84.5(4) . 2_656 ?
O4 Mn1 O1 122.6(4) 2_656 2_656 ?
O4 Mn1 O4 146.3(5) . 2_656 ?
O4 Mn1 O5 83.5(4) 2_656 2_656 ?
O4 Mn1 O5 80.2(4) 2_656 . ?
O4 Mn1 O5 80.2(4) . 2_656 ?
O4 Mn1 O5 83.5(4) . . ?
O5 Mn1 O1 84.6(4) . 2_656 ?
O5 Mn1 O1 84.6(4) 2_656 . ?
O5 Mn1 O1 147.6(4) 2_656 2_656 ?
O5 Mn1 O1 147.6(4) . . ?
O5 Mn1 O5 121.4(6) . 2_656 ?
H1A C1 H1B 108.2 . . ?
C0AA C1 H1A 109.8 2_656 . ?
C0AA C1 H1B 109.8 2_656 . ?
O4 C1 H1A 109.8 . . ?
O4 C1 H1B 109.8 . . ?
O4 C1 C0AA 109.4(12) . 2_656 ?
O1 Pb2 Br2 73.5(2) . . ?
O1 Pb2 Pb4 81.7(2) . . ?
O1 Pb2 O5 72.5(3) . 2_656 ?
Br2 Pb2 Pb4 117.07(3) . . ?
O3 Pb2 O1 74.9(3) . . ?
O3 Pb2 Br2 80.3(2) . . ?
O3 Pb2 Pb4 37.2(2) . . ?
O3 Pb2 O5 74.4(3) . 2_656 ?
O5 Pb2 Br2 141.7(2) 2_656 . ?
O5 Pb2 Pb4 40.6(2) 2_656 . ?
O1 C2 H2A 109.7 . . ?
O1 C2 H2B 109.7 . . ?
C2 C2 O1 110.0(10) 2_656 . ?
C2 C2 H2A 109.7 2_656 . ?
C2 C2 H2B 109.7 2_656 . ?
H2A C2 H2B 108.2 . . ?
Pb1 Br2 Pb2 92.10(4) . . ?
C1 C0AA H0AA 109.8 2_656 . ?
C1 C0AA H0AB 109.8 2_656 . ?
H0AA C0AA H0AB 108.2 . . ?
O5 C0AA C1 109.5(12) . 2_656 ?
O5 C0AA H0AA 109.8 . . ?
O5 C0AA H0AB 109.8 . . ?
O1 Pb3 Pb4 79.2(2) . . ?
O3 Pb3 O1 72.5(3) . . ?
O3 Pb3 Pb4 36.2(2) . . ?
O3 Pb3 O4 75.3(3) . 2_656 ?
O4 Pb3 O1 72.4(3) 2_656 . ?
O4 Pb3 Pb4 42.0(2) 2_656 . ?
Pb3 O3 Pb2 107.8(4) . . ?
Pb4 O3 Pb2 105.1(4) . . ?
Pb4 O3 Pb3 107.2(4) . . ?
Pb1 Br3 Pb1 148.66(13) 2_556 . ?
Pb2 Pb4 Pb3 60.999(16) . . ?
O3 Pb4 Pb2 37.7(3) . . ?
O3 Pb4 Pb3 36.6(2) . . ?
O3 Pb4 O4 73.5(3) . 2_656 ?
O3 Pb4 Br4 76.7(2) . 1_565 ?
O3 Pb4 O5 77.4(3) . 2_656 ?
O4 Pb4 Pb2 80.3(2) 2_656 . ?
O4 Pb4 Pb3 39.8(2) 2_656 . ?
O4 Pb4 Br4 137.4(2) 2_656 1_565 ?
Br4 Pb4 Pb2 57.72(3) 1_565 . ?
Br4 Pb4 Pb3 112.49(3) 1_565 . ?
O5 Pb4 Pb2 43.3(2) 2_656 . ?
O5 Pb4 Pb3 81.7(2) 2_656 . ?
O5 Pb4 O4 71.4(3) 2_656 2_656 ?
O5 Pb4 Br4 73.0(2) 2_656 1_565 ?
Mn1 O4 Pb3 102.6(4) . 2_656 ?
Mn1 O4 Pb4 100.6(4) . 2_656 ?
C1 O4 Mn1 109.8(9) . . ?
C1 O4 Pb3 119.2(8) . 2_656 ?
C1 O4 Pb4 123.3(9) . 2_656 ?
Pb3 O4 Pb4 98.2(4) 2_656 2_656 ?
Pb1 Br4 Pb4 110.20(5) . 1_545 ?
Pb1 Br5 Pb1 100.65(5) . 3_566 ?
Mn1 O5 Pb2 98.7(4) . 2_656 ?
Mn1 O5 Pb4 104.1(4) . 2_656 ?
C0AA O5 Mn1 110.0(8) . . ?
C0AA O5 Pb2 124.3(9) . 2_656 ?
C0AA O5 Pb4 120.1(8) . 2_656 ?
Pb4 O5 Pb2 96.1(3) 2_656 2_656 ?
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
Pb1 Br1 2.9662(15) . ?
Pb1 Br2 2.9451(16) . ?
Pb1 Br3 3.1068(11) . ?
Pb1 Br4 3.0406(15) . ?
Pb1 Br5 3.0403(18) . ?
Pb1 Br5 3.1173(16) 3_566 ?
O1 Mn1 2.156(10) . ?
O1 Pb2 2.368(10) . ?
O1 C2 1.467(16) . ?
O1 Pb3 2.499(10) . ?
Mn1 O1 2.156(10) 2_656 ?
Mn1 O4 2.140(10) 2_656 ?
Mn1 O4 2.140(10) . ?
Mn1 O5 2.144(10) . ?
Mn1 O5 2.144(10) 2_656 ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C0AA 1.52(2) 2_656 ?
C1 O4 1.458(18) . ?
Pb2 Br2 3.0784(15) . ?
Pb2 O3 2.311(10) . ?
Pb2 Pb4 3.6517(8) . ?
Pb2 O5 2.521(10) 2_656 ?
C2 C2 1.46(3) 2_656 ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C0AA C1 1.52(2) 2_656 ?
C0AA H0AA 0.9700 . ?
C0AA H0AB 0.9700 . ?
C0AA O5 1.434(18) . ?
Pb3 O3 2.307(9) . ?
Pb3 Pb4 3.6976(8) . ?
Pb3 O4 2.391(10) 2_656 ?
O3 Pb4 2.288(9) . ?
Br3 Pb1 3.1068(11) 2_556 ?
Pb4 O4 2.501(10) 2_656 ?
Pb4 Br4 3.1362(16) 1_565 ?
Pb4 O5 2.389(10) 2_656 ?
O4 Pb3 2.391(10) 2_656 ?
O4 Pb4 2.501(10) 2_656 ?
Br4 Pb4 3.1363(16) 1_545 ?
Br5 Pb1 3.1173(16) 3_566 ?
O5 Pb2 2.521(10) 2_656 ?
O5 Pb4 2.389(10) 2_656 ?
