Acylselenoureato bis(chelates) of lead: synthesis, structural characterization and microwave-assisted formation of PbSe nano- and microstructures
Klauke, Karsten; Schmitz, Alexa; Swertz, Ann-Christin; Beele, Björn B.; Giesen, Beatriz; Schlüsener, Carsten; Janiak, Christoph; Mohr, Fabian; New Journal of Chemistry 44 (2020) 7719–7726; doi:10.1039/D0NJ01433H

data_7059554
_publ_section_title
;
 Acylselenoureato bis(chelates) of lead: synthesis, structural
 characterization and microwave-assisted formation of PbSe nano- and
 microstructures
;
_journal_issue                   19
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              7719
_journal_page_last               7726
_journal_paper_doi               10.1039/D0NJ01433H
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C32 H44 Cl2 N4 O2 Pb Se2'
_chemical_formula_sum            'C32 H44 Cl2 N4 O2 Pb Se2'
_chemical_formula_weight         952.72
_space_group_crystal_system      orthorhombic
_space_group_IT_number           45
_space_group_name_Hall           'I 2 -2c'
_space_group_name_H-M_alt        'I b a 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_audit_creation_date             2017-11-17
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2020-01-27 deposited with the CCDC.	2020-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.9384(5)
_cell_length_b                   19.0184(12)
_cell_length_c                   10.4156(4)
_cell_measurement_reflns_used    2158
_cell_measurement_temperature    150
_cell_measurement_theta_max      29.3806
_cell_measurement_theta_min      3.1088
_cell_volume                     3553.4(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_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 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 16.2705
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.852
_diffrn_measurement_details
;
  1 omega  -78.00   38.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.5412    0.0000  -60.0000 116

  2 omega  -66.00  -33.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.5412  110.0000 -109.0000 33
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0123013000
_diffrn_orient_matrix_UB_12      0.0338142000
_diffrn_orient_matrix_UB_13      0.0194590000
_diffrn_orient_matrix_UB_21      0.0362670000
_diffrn_orient_matrix_UB_22      -0.0136905000
_diffrn_orient_matrix_UB_23      0.0110545000
_diffrn_orient_matrix_UB_31      0.0098573000
_diffrn_orient_matrix_UB_32      0.0079368000
_diffrn_orient_matrix_UB_33      -0.0642311000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0204
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.852
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5214
_diffrn_reflns_point_group_measured_fraction_full 0.826
_diffrn_reflns_point_group_measured_fraction_max 0.659
_diffrn_reflns_theta_full        25.050
_diffrn_reflns_theta_max         29.446
_diffrn_reflns_theta_min         3.115
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.981
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79542
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.781
_exptl_crystal_description       needle
_exptl_crystal_F_000             1856
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2/Hexanes'
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.580
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.100
_refine_ls_abs_structure_details
;
 Flack x determined using 884 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.069(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         3244
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0238
_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^)+(0.0203P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0465
_refine_ls_wR_factor_ref         0.0489
_reflns_Friedel_coverage         0.466
_reflns_Friedel_fraction_full    0.630
_reflns_Friedel_fraction_max     0.443
_reflns_number_gt                2931
_reflns_number_total             3244
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj01433h2.cif
_cod_data_source_block           kk110
_cod_depositor_comments
;Adding full bibliography for 7059550--7059554.cif.

 Adding full bibliography for 7059550--7059554.cif.
;
_cod_database_code               7059554
_shelxl_version_number           2013-3
_chemical_oxdiff_formula         C32H44O2Se2N4Cl2Pb1
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C10(H10), C14(H14)
2.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C13(H13A,H13B)
2.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C8(H8), C5(H5), C7(H7)
2.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C)
;
_shelx_res_checksum              35152
_olex2_date_sample_data_collection 2011-10-17
_olex2_submission_special_instructions 'No special instructions were received'