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_4128614
_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         'Cl14 Mn Pb4, 2(C5 H14 N2)'
_chemical_formula_sum            'C10 H28 Cl14 Mn N4 Pb4'
_chemical_formula_weight         1584.36
_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
_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                   10.3435(3)
_cell_length_b                   16.9247(6)
_cell_length_c                   18.3660(7)
_cell_measurement_reflns_used    6815
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      2.41
_cell_volume                     3215.16(19)
_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      200.15
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.962
_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  0.0697
_diffrn_reflns_av_unetI/netI     0.0705
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19997
_diffrn_reflns_point_group_measured_fraction_full 0.953
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         2.218
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    22.434
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.273
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             2828
_refine_diff_density_max         4.048
_refine_diff_density_min         -2.427
_refine_diff_density_rms         0.520
_refine_ls_abs_structure_details
;
 Flack x determined using 1962 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.024(10)
_refine_ls_extinction_coef       0.00125(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         6190
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0475
_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^)+(0.0727P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1145
_refine_ls_wR_factor_ref         0.1255
_reflns_Friedel_coverage         0.744
_reflns_Friedel_fraction_full    0.933
_reflns_Friedel_fraction_max     0.914
_reflns_number_gt                5399
_reflns_number_total             6190
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b04829_si_003.cif
_cod_data_source_block           2
_cod_database_code               4128614
_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 0.002 and sigma for 1-3 distances of 0.002
 C6, C7, C8, C9, C10, N3, N4
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim N1 \\sim N2: within 2A with sigma
of 0.002 and sigma for terminal atoms of 0.004
C6 \\sim C7 \\sim C8 \\sim C9 \\sim C10 \\sim N3 \\sim N4: within 2A with sigma
of 0.002 and sigma for terminal atoms of 0.004
4.a Ternary CH refined with riding coordinates:
 C6(H6), C1(H1)
4.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), N4(H4A,H4B), C8(H8A,H8B), C10(H10A,H10B), C9(H9A,H9B), C5(H5A,
 H5B), N2(H2A,H2B), C3(H3D,H3E), C4(H4C,H4D), C2(H2C,H2D)
4.c Idealised Me refined as rotating group:
 N3(H3A,H3B,H3C), N1(H1A,H1B,H1C)
;
_olex2_submission_special_instructions 'No special instructions were received'