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_7059550
_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         'C26 H34 N4 O2 Pb Se2'
_chemical_formula_sum            'C26 H34 N4 O2 Pb Se2'
_chemical_formula_weight         799.68
_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
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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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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                   20.7267(5)
_cell_length_b                   13.0349(11)
_cell_length_c                   10.1701(2)
_cell_measurement_reflns_used    2637
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      29.3314
_cell_measurement_theta_min      3.2013
_cell_volume                     2747.7(2)
_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
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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      150.0
_diffrn_detector_area_resol_mean 16.2705
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.849
_diffrn_measurement_details
;
  1 omega  -46.00  -20.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.3850  106.0000 -161.0000 26

  2 omega  -88.00   44.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.3850    0.0000  -60.0000 132
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0168259000
_diffrn_orient_matrix_UB_12      -0.0141898000
_diffrn_orient_matrix_UB_13      0.0578051000
_diffrn_orient_matrix_UB_21      -0.0149127000
_diffrn_orient_matrix_UB_22      -0.0408761000
_diffrn_orient_matrix_UB_23      -0.0344537000
_diffrn_orient_matrix_UB_31      0.0257339000
_diffrn_orient_matrix_UB_32      -0.0329030000
_diffrn_orient_matrix_UB_33      0.0178309000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0252
_diffrn_reflns_av_unetI/netI     0.0511
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.849
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4251
_diffrn_reflns_point_group_measured_fraction_full 0.812
_diffrn_reflns_point_group_measured_fraction_max 0.670
_diffrn_reflns_theta_full        25.050
_diffrn_reflns_theta_max         29.447
_diffrn_reflns_theta_min         3.212
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    8.820
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87688
_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    1.933
_exptl_crystal_description       block
_exptl_crystal_F_000             1536
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2/Hexanes'
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.831
_refine_diff_density_min         -0.700
_refine_diff_density_rms         0.117
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.007(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     162
_refine_ls_number_reflns         2543
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0254
_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^)+(0.0052P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0430
_refine_ls_wR_factor_ref         0.0461
_reflns_Friedel_coverage         0.495
_reflns_Friedel_fraction_full    0.602
_reflns_Friedel_fraction_max     0.470
_reflns_number_gt                2256
_reflns_number_total             2543
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj01433h2.cif
_cod_data_source_block           acspbsenet
_cod_depositor_comments
;Adding full bibliography for 7059550--7059554.cif.

 Adding full bibliography for 7059550--7059554.cif.
;
_cod_original_cell_volume        2747.7(3)
_cod_database_code               7059550
_shelxl_version_number           2013-3
_chemical_oxdiff_formula         C38H44N4Se3Pb1
_reflns_odcompleteness_completeness 99.57
_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 Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C3(H3A,H3B)
2.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C8(H8), C9(H9)
2.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C13(H13A,H13B,H13C), C2(H2A,H2B,H2C)
;
_shelx_res_checksum              75638
_olex2_date_sample_data_collection 2011-05-25
_olex2_submission_special_instructions 'No special instructions were received'