A Library of Selenourea Precursors to PbSe Nanocrystals with Size Distributions near the Homogeneous Limit.
Campos, Michael P.; Hendricks, Mark P.; Beecher, Alexander N.; Walravens, Willem; Swain, Robert A.; Cleveland, Gregory T.; Hens, Zeger; Sfeir, Matthew Y.; Owen, Jonathan S.; Journal of the American Chemical Society 139 (2017) 2296–2305; doi:10.1021/jacs.6b11021

data_4125572
_publ_section_title
;
 A Library of Selenourea Precursors to PbSe Nanocrystals with Size
 Distributions near the Homogeneous Limit.
;
_journal_issue                   6
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2296
_journal_page_last               2305
_journal_paper_doi               10.1021/jacs.6b11021
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         'C11 H22 N2 Se'
_chemical_formula_sum            'C11 H22 N2 Se'
_chemical_formula_weight         261.26
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-01-11
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.94407(19)
_cell_length_b                   9.68682(10)
_cell_length_c                   6.18700(6)
_cell_measurement_reflns_used    16147
_cell_measurement_temperature    99.9(4)
_cell_measurement_theta_max      71.4210
_cell_measurement_theta_min      4.9800
_cell_volume                     1255.23(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_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_environment      N~2~
_diffrn_ambient_temperature      99.9(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0549
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega    1.00   74.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.5316  -99.0000  120.0000 73

  2 omega  -34.00   55.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.5316  -37.0000   90.0000 89

  3 omega    9.00  103.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.5316   77.0000   30.0000 94

  4 omega    1.00   74.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.5316  -99.0000    0.0000 73

  5 omega   19.00  103.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.5316   57.0000    0.0000 84

  6 omega    9.00  103.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.5316   77.0000 -120.0000 94

  7 omega   19.00  103.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.5316   57.0000 -150.0000 84

  8 omega    9.00  103.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.5316   77.0000  -60.0000 94

  9 omega   40.00   99.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -30.0000 59

 10 omega   38.00   91.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -150.0000 53

 11 omega   37.00  137.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -19.0000   54.3269 100

 12 omega   40.00   99.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000   30.0000 59

 13 omega   39.00  109.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000  -90.0000 70

 14 omega   38.00  116.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000 -150.0000 78

 15 omega   91.00  176.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000   60.0000 85

 16 omega   38.00   91.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   30.0000 53

 17 omega   37.00  146.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -15.0000  -60.0000 109

 18 omega   70.00  178.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000    0.0000 108

 19 omega   39.00  109.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000  -60.0000 70

 20 omega   40.00   99.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000 -180.0000 59

 21 omega   38.00  116.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000 -120.0000 78

 22 omega  100.00  178.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000   60.0000 78

 23 omega   38.00  116.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000   60.0000 78

 24 omega   38.00  116.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000    0.0000 78

 25 omega   38.00  116.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  120.0000 78

 26 omega   40.00  135.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000  150.0000 95

 27 omega   70.00  178.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000  -60.0000 108

 28 omega   40.00   99.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000   60.0000 59

 29 omega   38.00   91.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -120.0000 53

 30 omega  100.00  178.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000  -90.0000 78

 31 omega   41.00  126.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -61.0000  -30.0000 85

 32 omega   38.00   91.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   90.0000 53

 33 omega   40.00  135.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000   90.0000 95

 34 omega   40.00   99.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  120.0000 59

 35 omega   39.00  109.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000 -120.0000 70

 36 omega   39.00  109.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000   60.0000 70

 37 omega   39.00  109.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000  120.0000 70

 38 omega  100.00  178.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000  120.0000 78

 39 omega   91.00  176.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000 -120.0000 85

 40 omega   91.00  176.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000   30.0000 85

 41 omega   40.00  135.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000  -90.0000 95

 42 omega   40.00  135.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000   60.0000 95

 43 omega   38.00   92.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -26.0000 -106.7021 54

 44 omega    1.00   74.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.5316  -99.0000   90.0000 73

 45 omega  -32.00   62.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.5316  -77.0000 -150.0000 94

 46 omega   57.00  108.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.5316  178.0000  -30.0000 51

 47 omega   16.00  105.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.5316   37.0000  150.0000 89

 48 omega    9.00  103.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.5316   77.0000  150.0000 94

 49 omega  -32.00   52.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.5316  -57.0000  -90.0000 84

 50 omega   -2.00   24.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.5316   96.0000   71.0828 26

 51 omega    0.00   27.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.5316   93.0000   -0.7653 27

 52 omega    9.00  103.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.5316   77.0000   60.0000 94

 53 omega  -34.00   55.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.5316  -37.0000  -30.0000 89

 54 omega   81.00  176.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -30.0000 95

 55 omega   87.00  178.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000 -180.0000 91

 56 omega   87.00  178.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000 -150.0000 91

 57 omega   81.00  176.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -90.0000 95

 58 omega   70.00  178.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000  150.0000 108

 59 omega   81.00  176.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0199165000
_diffrn_orient_matrix_UB_12      -0.1530118000
_diffrn_orient_matrix_UB_13      0.0078315000
_diffrn_orient_matrix_UB_21      0.0605257000
_diffrn_orient_matrix_UB_22      -0.0394814000
_diffrn_orient_matrix_UB_23      -0.1272607000
_diffrn_orient_matrix_UB_31      0.0367309000
_diffrn_orient_matrix_UB_32      -0.0179040000
_diffrn_orient_matrix_UB_33      0.2139183000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0802
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            28148
_diffrn_reflns_point_group_measured_fraction_full 0.941
_diffrn_reflns_point_group_measured_fraction_max 0.939
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.498
_diffrn_reflns_theta_min         5.030
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.776
_exptl_absorpt_correction_T_max  0.898
_exptl_absorpt_correction_T_min  0.578
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_description
;
;
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.2869
_exptl_crystal_size_mid          0.0461
_exptl_crystal_size_min          0.034
_refine_diff_density_max         0.913
_refine_diff_density_min         -0.500
_refine_diff_density_rms         0.105
_refine_ls_abs_structure_details
;
 Flack x determined using 900 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.05(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     133
_refine_ls_number_reflns         2294
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0394
_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^)+(0.0820P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0990
_refine_ls_wR_factor_ref         0.1001
_reflns_Friedel_coverage         0.712
_reflns_Friedel_fraction_full    0.870
_reflns_Friedel_fraction_max     0.865
_reflns_number_gt                2238
_reflns_number_total             2294
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            14.cif
_cod_data_source_block           wcorr
_cod_depositor_comments
'Adding full bibliography for 4125565--4125579.cif.'
_cod_database_code               4125572
_chemical_oxdiff_formula         'C44 H88 N8 Se4'
_chemical_oxdiff_usercomment     'Colorless needles'
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Restrained distances
 N3-H3
 0.88 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C4(H4), C11(H11)
3.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B)
3.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              83178
_shelx_hkl_checksum              48939
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'