#------------------------------------------------------------------------------
#$Date: 2020-12-09 04:14:26 +0100 (Wed 09 de Dec de 2020) $
#$Revision: 259693 $
#$URL: svn://www.crystallography.net/cod/cif/7/70/58/7705874.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_7705874
loop_
_publ_author_name
'Yu, Shan-Shan'
'Zhao, Hai-Rong'
'Zhang, Hui'
'Duan, Hai-Bao'
_publ_section_title
;
 Two chiral haloplumbate hybrids with thermochromism luminescence and
 application potential as luminescent thermometers.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16643
_journal_page_last               16648
_journal_paper_doi               10.1039/d0dt02261f
_journal_volume                  49
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'Cl4 Pb, C6 H16 N2'
_chemical_formula_sum            'C6 H16 Cl4 N2 Pb'
_chemical_formula_weight         465.20
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-03-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-06-23 deposited with the CCDC.	2020-10-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.7465(6)
_cell_length_b                   13.5915(9)
_cell_length_c                   16.9107(11)
_cell_measurement_reflns_used    3210
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      28.9010
_cell_measurement_theta_min      2.8380
_cell_volume                     1780.5(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (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      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2684
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -38.00  68.00   1.00    2.67    --  -11.59  19.00 120.00  106
  2  ω     26.00  59.00   1.00    2.67    --   11.74  37.00-180.00   33
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0225631000
_diffrn_orient_matrix_UB_12      -0.0349095000
_diffrn_orient_matrix_UB_13      -0.0294116000
_diffrn_orient_matrix_UB_21      -0.0341916000
_diffrn_orient_matrix_UB_22      -0.0314779000
_diffrn_orient_matrix_UB_23      0.0295863000
_diffrn_orient_matrix_UB_31      -0.0818747000
_diffrn_orient_matrix_UB_32      0.0227482000
_diffrn_orient_matrix_UB_33      -0.0041695000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_unetI/netI     0.0760
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            5525
_diffrn_reflns_point_group_measured_fraction_full 0.951
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        24.995
_diffrn_reflns_theta_max         24.995
_diffrn_reflns_theta_min         1.922
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    10.049
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30843
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (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    1.735
_exptl_crystal_description       block
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.415
_refine_diff_density_min         -4.556
_refine_diff_density_rms         0.339
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.107(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         2978
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0641
_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)+(0.0279P)²+94.4011P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1431
_refine_ls_wR_factor_ref         0.1477
_reflns_Friedel_coverage         0.642
_reflns_Friedel_fraction_full    0.884
_reflns_Friedel_fraction_max     0.884
_reflns_number_gt                2850
_reflns_number_total             2978
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt02261f2.cif
_cod_data_source_block           03-2
_cod_database_code               7705874
_shelx_shelxl_version_number     2018/3
_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   0.500
_shelx_estimated_absorpt_t_min   0.404
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.893(16)
 0.107(16)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
3. Rigid bond restraints
 C1, C2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2: within 2A with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq: with sigma of 0.002 and sigma
for terminal atoms of 0.004
Uanis(N1) \\sim Ueq, Uanis(N2) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
5.a Ternary CH refined with riding coordinates:
 C6(H6), C1(H1)
5.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C3(H3A,H3B), C4(H4A,H4B), C2(H2D,H2E)
5.c Idealised Me refined as rotating group:
 N2(H2A,H2B,H2C), N1(H1A,H1B,H1C)
;
_olex2_date_sample_data_collection 2019-03-21
_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 2.107
_oxdiff_exptl_absorpt_empirical_full_min 0.701
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -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
Pb01 Pb 0.30688(7) 0.70277(3) 0.37667(3) 0.01153(10) Uani 1 1 d . . . . .
Cl1 Cl -0.0079(5) 0.6598(3) 0.3055(2) 0.0222(10) Uani 1 1 d . . . . .
Cl2 Cl 0.4723(5) 0.6530(3) 0.24474(19) 0.0164(9) Uani 1 1 d . . . . .
Cl3 Cl 0.3241(5) 0.5071(2) 0.4332(2) 0.0207(9) Uani 1 1 d . . . . .
Cl4 Cl 0.6429(5) 0.7361(3) 0.4569(2) 0.0268(11) Uani 1 1 d . . . . .
C6 C 0.8061(17) 0.4365(8) 0.3861(7) 0.0068(12) Uani 1 1 d . U . . .
H6 H 0.922522 0.434356 0.363485 0.008 Uiso 1 1 calc R . . . .
N2 N 0.7034(16) 0.5085(8) 0.3411(6) 0.0136(19) Uani 1 1 d . U . . .
H2A H 0.681586 0.484864 0.293061 0.016 Uiso 1 1 calc GR . . . .
H2B H 0.762301 0.564531 0.336872 0.016 Uiso 1 1 calc GR . . . .
H2C H 0.604372 0.519788 0.366186 0.016 Uiso 1 1 calc GR . . . .
C5 C 0.7214(17) 0.3366(9) 0.3732(9) 0.0163(12) Uani 1 1 d . U . . .
H5A H 0.600949 0.339819 0.388743 0.020 Uiso 1 1 calc R . . . .
H5B H 0.726254 0.319490 0.317564 0.020 Uiso 1 1 calc R . . . .
C3 C 0.821(2) 0.2833(11) 0.5096(8) 0.0220(13) Uani 1 1 d . U . . .
H3A H 0.706052 0.285297 0.531966 0.026 Uiso 1 1 calc R . . . .
H3B H 0.886908 0.233025 0.537069 0.026 Uiso 1 1 calc R . . . .
C1 C 0.8209(19) 0.4632(9) 0.4730(7) 0.0079(7) Uani 1 1 d . U . . .
H1 H 0.704310 0.472651 0.494193 0.009 Uiso 1 1 calc R . . . .
C4 C 0.812(2) 0.2593(11) 0.4209(9) 0.0250(13) Uani 1 1 d . U . . .
H4A H 0.928187 0.251261 0.400687 0.030 Uiso 1 1 calc R . . . .
H4B H 0.752055 0.197131 0.414113 0.030 Uiso 1 1 calc R . . . .
N1 N 0.9194(15) 0.5556(8) 0.4848(7) 0.0103(19) Uani 1 1 d . U . . .
H1A H 0.852727 0.606821 0.472934 0.012 Uiso 1 1 calc GR . . . .
H1B H 1.011792 0.555533 0.453497 0.012 Uiso 1 1 calc GR . . . .
H1C H 0.952911 0.559853 0.535024 0.012 Uiso 1 1 calc GR . . . .
C2 C 0.9074(17) 0.3815(9) 0.5192(8) 0.0083(7) Uani 1 1 d . U . . .
H2D H 1.026549 0.376086 0.502135 0.010 Uiso 1 1 calc R . . . .
H2E H 0.907820 0.398890 0.574849 0.010 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'
Cl Cl 0.1484 0.1585 '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'
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
Cl1 Pb01 Cl3 89.44(11) . . ?
Cl1 Pb01 Cl4 176.44(11) . . ?
Cl2 Pb01 Cl1 90.36(12) . . ?
Cl2 Pb01 Cl3 91.25(11) . . ?
Cl2 Pb01 Cl4 89.98(11) . . ?
Cl3 Pb01 Cl4 87.01(11) . . ?
N2 C6 H6 108.4 . . ?
N2 C6 C5 106.6(10) . . ?
N2 C6 C1 112.4(10) . . ?
C5 C6 H6 108.4 . . ?
C1 C6 H6 108.4 . . ?
C1 C6 C5 112.6(11) . . ?
C6 N2 H2A 109.5 . . ?
C6 N2 H2B 109.5 . . ?
C6 N2 H2C 109.5 . . ?
H2A N2 H2B 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
C6 C5 H5A 109.6 . . ?
C6 C5 H5B 109.6 . . ?
H5A C5 H5B 108.1 . . ?
C4 C5 C6 110.3(12) . . ?
C4 C5 H5A 109.6 . . ?
C4 C5 H5B 109.6 . . ?
H3A C3 H3B 108.4 . . ?
C4 C3 H3A 110.0 . . ?
C4 C3 H3B 110.0 . . ?
C2 C3 H3A 110.0 . . ?
C2 C3 H3B 110.0 . . ?
C2 C3 C4 108.4(12) . . ?
C6 C1 H1 108.4 . . ?
N1 C1 C6 111.8(10) . . ?
N1 C1 H1 108.4 . . ?
N1 C1 C2 108.9(11) . . ?
C2 C1 C6 110.9(10) . . ?
C2 C1 H1 108.4 . . ?
C5 C4 C3 113.5(13) . . ?
C5 C4 H4A 108.9 . . ?
C5 C4 H4B 108.9 . . ?
C3 C4 H4A 108.9 . . ?
C3 C4 H4B 108.9 . . ?
H4A C4 H4B 107.7 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C3 C2 C1 113.6(11) . . ?
C3 C2 H2D 108.8 . . ?
C3 C2 H2E 108.8 . . ?
C1 C2 H2D 108.8 . . ?
C1 C2 H2E 108.8 . . ?
H2D C2 H2E 107.7 . . ?
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
Pb01 Cl1 2.781(4) . ?
Pb01 Cl2 2.660(3) . ?
Pb01 Cl3 2.829(3) . ?
Pb01 Cl4 2.970(4) . ?
C6 H6 0.9800 . ?
C6 N2 1.473(16) . ?
C6 C5 1.523(17) . ?
C6 C1 1.519(17) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 H2C 0.8900 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C4 1.50(2) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.54(2) . ?
C3 C2 1.50(2) . ?
C1 H1 0.9800 . ?
C1 N1 1.482(17) . ?
C1 C2 1.514(18) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
C2 H2D 0.9700 . ?
C2 H2E 0.9700 . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.893(16)
2 0.107(16)
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.577 0.186 0.250 291.5 91.7 ?
2 -0.608 0.069 0.750 291.5 102.3 ?
