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_7059552
_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      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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
;
2020-01-27 deposited with the CCDC.	2020-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.813(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6871(5)
_cell_length_b                   15.8440(6)
_cell_length_c                   10.4873(4)
_cell_measurement_reflns_used    4218
_cell_measurement_temperature    150
_cell_measurement_theta_max      29.2370
_cell_measurement_theta_min      3.1128
_cell_volume                     1724.42(13)
_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 0.998
_diffrn_measured_fraction_theta_max 0.837
_diffrn_measurement_details
;
  1 omega    5.00   76.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       17.8225   77.0000  -30.0000 71

  2 omega  -43.00   80.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       17.8225    0.0000  -60.0000 123

  3 omega  -11.00   48.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.3850   77.0000   90.0000 59
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0596677000
_diffrn_orient_matrix_UB_12      0.0218066000
_diffrn_orient_matrix_UB_13      -0.0145498000
_diffrn_orient_matrix_UB_21      0.0045830000
_diffrn_orient_matrix_UB_22      0.0055171000
_diffrn_orient_matrix_UB_23      0.0680916000
_diffrn_orient_matrix_UB_31      0.0329361000
_diffrn_orient_matrix_UB_32      0.0387242000
_diffrn_orient_matrix_UB_33      -0.0014938000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_av_unetI/netI     0.0346
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.837
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            8277
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.837
_diffrn_reflns_theta_full        25.050
_diffrn_reflns_theta_max         29.302
_diffrn_reflns_theta_min         3.235
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    2.333
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90977
_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    1.440
_exptl_crystal_description       cube
_exptl_crystal_F_000             768
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: EtOH'
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.729
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         3951
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0314
_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^)+(0.0298P)^2^+1.4217P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0712
_refine_ls_wR_factor_ref         0.0758
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3392
_reflns_number_total             3951
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj01433h2.cif
_cod_data_source_block           kk007
_cod_depositor_comments
;Adding full bibliography for 7059550--7059554.cif.

 Adding full bibliography for 7059550--7059554.cif.
;
_cod_original_cell_volume        1724.43(12)
_cod_database_code               7059552
_shelxl_version_number           2013-3
_chemical_oxdiff_formula         C16H14Cl1O1Se1N2
_reflns_odcompleteness_completeness 99.75
_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 Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C15(H15A,H15B), C9(H9A,H9B), C11(H11A,H11B), C10(H10A,H10B),
 C14(H14A,H14B)
2.b Aromatic/amide H refined with riding coordinates:
 C8(H8), N1(H1), C4(H4), C7(H7), C5(H5)
2.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              43773
_olex2_date_sample_data_collection 2011-09-06
_olex2_submission_special_instructions 'No special instructions were received'