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_7059551
_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         'C16 H23 Cl N2 O Se'
_chemical_formula_sum            'C16 H23 Cl N2 O Se'
_chemical_formula_weight         373.77
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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)
;
_audit_update_record
;
2020-01-27 deposited with the CCDC.	2020-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                64.775(8)
_cell_angle_beta                 69.712(8)
_cell_angle_gamma                80.596(6)
_cell_formula_units_Z            2
_cell_length_a                   8.1942(7)
_cell_length_b                   10.8431(8)
_cell_length_c                   11.8118(12)
_cell_measurement_reflns_used    3250
_cell_measurement_temperature    149.9
_cell_measurement_theta_max      29.3607
_cell_measurement_theta_min      2.9151
_cell_volume                     890.36(15)
_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
_diffrn_detector_area_resol_mean 16.2705
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.826
_diffrn_measurement_details
;
  1 omega   26.00   53.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.9787   77.0000  -90.0000 27

  2 omega   -6.00   20.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.9787   81.0000  106.0000 26

  3 omega  -26.00   48.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.9787    0.0000  -60.0000 74

  4 omega  -90.00   11.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.5412  -77.0000  -30.0000 101

  5 omega  -45.00   50.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.5412   77.0000 -120.0000 95

  6 omega  -82.00   11.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.5412  -77.0000  120.0000 93
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0844638000
_diffrn_orient_matrix_UB_12      0.0046893000
_diffrn_orient_matrix_UB_13      0.0425264000
_diffrn_orient_matrix_UB_21      -0.0372251000
_diffrn_orient_matrix_UB_22      -0.0071242000
_diffrn_orient_matrix_UB_23      -0.0428393000
_diffrn_orient_matrix_UB_31      -0.0001117000
_diffrn_orient_matrix_UB_32      -0.0718176000
_diffrn_orient_matrix_UB_33      0.0351078000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.826
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7450
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.826
_diffrn_reflns_theta_full        25.050
_diffrn_reflns_theta_max         29.425
_diffrn_reflns_theta_min         2.921
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    2.259
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77286
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_description       plate
_exptl_crystal_F_000             384
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: EtOH'
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.547
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         4067
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0320
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0225P)^2^+0.2843P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0661
_refine_ls_wR_factor_ref         0.0699
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3604
_reflns_number_total             4067
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj01433h2.cif
_cod_data_source_block           kk010_1
_cod_depositor_comments
;Adding full bibliography for 7059550--7059554.cif.

 Adding full bibliography for 7059550--7059554.cif.
;
_cod_database_code               7059551
_shelxl_version_number           2013-3
_chemical_oxdiff_formula         C16H19O1N2Se1Cl1
_reflns_odcompleteness_completeness 99.86
_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, All N(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:
 C13(H13A,H13B), C9(H9A,H9B)
2.c Aromatic/amide H refined with riding coordinates:
 N1(H1), 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              56913
_olex2_date_sample_data_collection 2011-09-27
_olex2_submission_special_instructions 'No special instructions were received'