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_7059553
_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 H28 N6 O6 Pb Se2'
_chemical_formula_sum            'C32 H28 N6 O6 Pb Se2'
_chemical_formula_weight         957.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-11-17
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Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
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_audit_update_record
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2017-11-21 deposited with the CCDC.	2020-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.0944(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_length_b                   14.1942(2)
_cell_length_c                   16.5168(2)
_cell_measurement_reflns_used    6569
_cell_measurement_temperature    150
_cell_measurement_theta_max      29.3402
_cell_measurement_theta_min      3.0314
_cell_volume                     3309.80(8)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_reduction
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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 0.991
_diffrn_measured_fraction_theta_max 0.823
_diffrn_measurement_details
;
  1 omega  -87.00   11.00   1.0000  125.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.3850  -77.0000 -150.0000 98

  2 omega  -72.00   35.00   1.0000  125.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.3850    0.0000    0.0000 107
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0383736000
_diffrn_orient_matrix_UB_12      -0.0077614000
_diffrn_orient_matrix_UB_13      0.0298242000
_diffrn_orient_matrix_UB_21      -0.0278615000
_diffrn_orient_matrix_UB_22      0.0169785000
_diffrn_orient_matrix_UB_23      0.0305052000
_diffrn_orient_matrix_UB_31      -0.0166251000
_diffrn_orient_matrix_UB_32      -0.0463528000
_diffrn_orient_matrix_UB_33      0.0061707000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_unetI/netI     0.0435
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.823
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13648
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.823
_diffrn_reflns_theta_full        25.050
_diffrn_reflns_theta_max         29.405
_diffrn_reflns_theta_min         3.105
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    7.350
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61767
_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    1.922
_exptl_crystal_description       needle
_exptl_crystal_F_000             1840
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2/Hexane'
_exptl_crystal_size_max          0.08
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_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.492
_refine_diff_density_min         -1.247
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         7523
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0308
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0315P)^2^+0.0568P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0646
_refine_ls_wR_factor_ref         0.0700
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6269
_reflns_number_total             7523
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj01433h2.cif
_cod_data_source_block           acspbsemear
_cod_depositor_comments
;Adding full bibliography for 7059550--7059554.cif.

 Adding full bibliography for 7059550--7059554.cif.
;
_cod_original_cell_volume        3309.79(9)
_cod_database_code               7059553
_shelxl_version_number           2013-3
_chemical_oxdiff_formula         C30H28N6O2Se2Pb1
_reflns_odcompleteness_completeness 98.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C19(H19), C23(H23), C32(H32), C22(H22), C31(H31), C3(H3), C4(H4), C29(H29),
 C16(H16), C7(H7), C28(H28), C12(H12), C6(H6), C15(H15), C13(H13), C20(H20)
2.b Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C1(H1A,H1B,H1C), C17(H17A,H17B,H17C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              54323
_olex2_date_sample_data_collection 2011-05-24
_olex2_submission_special_instructions 'No special instructions were received'