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_4125570
_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         'C9 H18 N2 Se'
_chemical_formula_sum            'C9 H18 N2 Se'
_chemical_formula_weight         233.21
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-12-31
_audit_creation_method
;
Olex2 1.2
(compiled 2014.12.23 svn.r3118 for OlexSys, GUI svn.r4975)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.1599(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.58561(17)
_cell_length_b                   10.51744(17)
_cell_length_c                   9.66073(16)
_cell_measurement_reflns_used    11658
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.9320
_cell_measurement_theta_min      3.8580
_cell_volume                     1069.35(3)
_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, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0549
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_details
;
  1 omega  -52.00   36.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1930  -37.0000   60.0000 88

  2 omega   35.00   89.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1930  178.0000    0.0000 54

  3 omega  -12.00   89.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1930   19.0000 -120.0000 101

  4 omega   34.00   90.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1930 -178.0000  -90.0000 56

  5 omega    0.00   84.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1930   57.0000  150.0000 84

  6 omega    0.00   84.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1930   57.0000  -60.0000 84

  7 omega  -20.00   56.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1930  -99.0000    0.0000 76

  8 omega  -20.00   56.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1930  -99.0000 -120.0000 76

  9 omega  -10.00   85.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1930   77.0000   30.0000 95

 10 omega  -20.00   56.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1930  -99.0000   60.0000 76

 11 omega    0.00   84.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1930   57.0000 -120.0000 84

 12 omega   35.00   89.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1930  178.0000   30.0000 54

 13 omega  -20.00   56.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1930  -99.0000 -180.0000 76

 14 omega  -20.00   56.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1930  -99.0000  -90.0000 76

 15 omega  -50.00   44.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1930  -77.0000  150.0000 94

 16 omega  -20.00   52.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1930  -99.0000   90.0000 72
;
_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      -0.0012803000
_diffrn_orient_matrix_UB_12      -0.0037587000
_diffrn_orient_matrix_UB_13      0.0731456000
_diffrn_orient_matrix_UB_21      -0.0565406000
_diffrn_orient_matrix_UB_22      -0.0365622000
_diffrn_orient_matrix_UB_23      -0.0100283000
_diffrn_orient_matrix_UB_31      0.0366490000
_diffrn_orient_matrix_UB_32      -0.0565477000
_diffrn_orient_matrix_UB_33      0.0016523000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            29160
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.624
_diffrn_reflns_theta_min         3.334
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.465
_exptl_absorpt_correction_T_max  0.796
_exptl_absorpt_correction_T_min  0.537
_exptl_absorpt_correction_type   analytical
_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)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_description
;
;
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.2505
_exptl_crystal_size_mid          0.1828
_exptl_crystal_size_min          0.0791
_refine_diff_density_max         0.399
_refine_diff_density_min         -0.282
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     114
_refine_ls_number_reflns         2832
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0238
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0205P)^2^+0.4816P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0489
_refine_ls_wR_factor_ref         0.0507
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2554
_reflns_number_total             2832
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            22.cif
_cod_data_source_block           wcorr
_cod_depositor_comments
'Adding full bibliography for 4125565--4125579.cif.'
_cod_database_code               4125570
_chemical_oxdiff_formula         'C36 H72 N8 Se4'
_reflns_odcompleteness_completeness 99.70
_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. Restrained distances
 N3-H3
 0.88 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C4(H4)
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:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              40905
_shelx_hkl_checksum              90169
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'