Tailored Synthesis of an Unprecedented Pb-Mn Heterometallic Halide Hybrid with Enhanced Emission.
Peng, Yu; Li, Lina; Ji, Chengmin; Wu, Zhenyue; Wang, Sasa; Liu, Xitao; Yao, Yunpeng; Luo, Junhua; Journal of the American Chemical Society 141 (2019) 12197–12201; doi:10.1021/jacs.9b04829

data_4128613
_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       '\f and \w 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/[\s^2^(Fo^2^)+(0.0420P)^2^] where P=(Fo^2^+2Fc^2^)/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 > 2\s(I)'
_cod_data_source_file            ja9b04829_si_002.cif
_cod_data_source_block           1
_cod_database_code               4128613
_shelx_shelxl_version_number     2017/1
_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'