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_4125566
_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 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-01-01
_audit_creation_method
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Olex2 1.2
(compiled 2014.12.23 svn.r3118 for OlexSys, GUI svn.r4975)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.004(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.2032(2)
_cell_length_b                   9.9913(5)
_cell_length_c                   17.2951(7)
_cell_measurement_reflns_used    3408
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.5770
_cell_measurement_theta_min      3.8420
_cell_volume                     1071.26(8)
_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
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
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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      100.15
_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 0.884
_diffrn_measurement_details
;
  1 omega   35.00   89.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1930  178.0000    0.0000 54

  2 omega  -52.00   86.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1930    0.0000 -180.0000 138

  3 omega  -50.00   44.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1930  -77.0000    0.0000 94

  4 omega  -82.00   12.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.6148  -77.0000   90.0000 94

  5 omega  -82.00    2.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.6148  -57.0000 -180.0000 84

  6 omega    0.00   19.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1930   57.0000   60.0000 19
;
_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      -0.0999716000
_diffrn_orient_matrix_UB_12      -0.0024154000
_diffrn_orient_matrix_UB_13      0.0186797000
_diffrn_orient_matrix_UB_21      0.0284370000
_diffrn_orient_matrix_UB_22      0.0586926000
_diffrn_orient_matrix_UB_23      0.0210143000
_diffrn_orient_matrix_UB_31      -0.0478986000
_diffrn_orient_matrix_UB_32      0.0398221000
_diffrn_orient_matrix_UB_33      -0.0298948000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_unetI/netI     0.0444
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.884
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            11134
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.884
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.591
_diffrn_reflns_theta_min         3.452
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.459
_exptl_absorpt_correction_T_max  0.931
_exptl_absorpt_correction_T_min  0.794
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
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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    1.446
_exptl_crystal_description
;
;
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.0858
_exptl_crystal_size_mid          0.0475
_exptl_crystal_size_min          0.0268
_refine_diff_density_max         0.563
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         2661
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0350
_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^)+(0.0177P)^2^+0.7545P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0602
_refine_ls_wR_factor_ref         0.0639
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2255
_reflns_number_total             2661
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            31.cif
_cod_data_source_block           w1corr
_cod_depositor_comments
'Adding full bibliography for 4125565--4125579.cif.'
_cod_database_code               4125566
_chemical_oxdiff_formula         'C36 H72 N8 Se4'
_chemical_oxdiff_usercomment     Block
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N10-H10
 0.88 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B)
3.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              39821
_shelx_hkl_checksum              88197
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'