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_4125568
_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           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-01-01
_audit_creation_method
;
Olex2 1.2
(compiled 2014.12.23 svn.r3118 for OlexSys, GUI svn.r4975)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9340(3)
_cell_length_b                   9.8566(3)
_cell_length_c                   11.2837(3)
_cell_measurement_reflns_used    7209
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.2820
_cell_measurement_theta_min      3.9730
_cell_volume                     1327.29(6)
_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 0.957
_diffrn_measurement_details
;
  1 omega   -2.00   86.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1930   37.0000  -60.0000 88

  2 omega  -20.00   56.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1930  -99.0000   90.0000 76

  3 omega   -2.00   86.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1930   37.0000    0.0000 88

  4 omega  -55.00   -4.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.6148  101.0000  -38.0000 51

  5 omega  -61.00  -13.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.6148  112.0000 -137.0000 48

  6 omega   -2.00   86.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1930   37.0000 -150.0000 88

  7 omega  -50.00   34.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1930  -57.0000 -180.0000 84

  8 omega  -10.00   85.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1930   77.0000   90.0000 95

  9 omega   35.00   89.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1930  178.0000    0.0000 54

 10 omega  -20.00   56.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1930  -99.0000 -180.0000 76

 11 omega    0.00   63.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1930   57.0000    0.0000 63

 12 omega   35.00   89.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1930  178.0000   60.0000 54
;
_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      0.0115220000
_diffrn_orient_matrix_UB_12      -0.0705870000
_diffrn_orient_matrix_UB_13      0.0004224000
_diffrn_orient_matrix_UB_21      0.0175080000
_diffrn_orient_matrix_UB_22      0.0046904000
_diffrn_orient_matrix_UB_23      0.0599589000
_diffrn_orient_matrix_UB_31      -0.0556220000
_diffrn_orient_matrix_UB_32      -0.0131459000
_diffrn_orient_matrix_UB_33      0.0188817000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0689
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            24645
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.921
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.524
_diffrn_reflns_theta_min         3.414
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.800
_exptl_absorpt_correction_T_max  0.926
_exptl_absorpt_correction_T_min  0.448
_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    1.307
_exptl_crystal_description
;
;
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.4621
_exptl_crystal_size_mid          0.0808
_exptl_crystal_size_min          0.0356
_refine_diff_density_max         0.363
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details
;
 Flack x determined using 1137 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.011(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     132
_refine_ls_number_reflns         3424
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0344
_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^)+(0.0170P)^2^+0.4560P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0583
_refine_ls_wR_factor_ref         0.0616
_reflns_Friedel_coverage         0.835
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.882
_reflns_number_gt                2926
_reflns_number_total             3424
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            17.cif
_cod_data_source_block           wcorr
_cod_depositor_comments
'Adding full bibliography for 4125565--4125579.cif.'
_cod_original_cell_volume        1327.29(7)
_cod_database_code               4125568
_chemical_oxdiff_formula         'C44 H88 N8 Se4'
_chemical_oxdiff_usercomment     'Big, flat needle'
_reflns_odcompleteness_completeness 99.56
_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
 N10-H10
 0.88 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C11(H11)
3.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C6(H6A,H6B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B),
 C15(H15A,H15B), C16(H16A,H16B)
3.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C7(H7A,H7B,H7C)
;
_shelx_res_checksum              22161
_shelx_hkl_checksum              7535
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'