#------------------------------------------------------------------------------
#$Date: 2019-11-26 05:08:11 +0200 (Tue, 26 Nov 2019) $
#$Revision: 242668 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/27/4132760.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4132760
loop_
_publ_author_name
'Mullane, Kimberly C.'
'Ryu, Ho'
'Cheisson, Thibault'
'Grant, Lauren N.'
'Park, Ji Young'
'Manor, Brian C.'
'Carroll, Patrick J.'
'Baik, Mu-Hyun'
'Mindiola, Daniel J.'
'Schelter, Eric J.'
_publ_section_title
;
 C-H Bond Addition across a Transient Uranium-Nitrido Moiety and Formation
 of a Parent Uranium Imido Complex.
;
_journal_issue                   36
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11335
_journal_page_last               11340
_journal_paper_doi               10.1021/jacs.8b06090
_journal_volume                  140
_journal_year                    2018
_chemical_formula_sum            'C44 H62 I N2 P2 U'
_chemical_formula_weight         1045.83
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      18
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.4461(4)
_cell_length_b                   15.3301(5)
_cell_length_c                   11.6893(3)
_cell_measurement_reflns_used    9941
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.39
_cell_volume                     2230.32(12)
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'CCD Area Detector'
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_sigmaI/netI    0.0501
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            25438
_diffrn_reflns_theta_full        27.60
_diffrn_reflns_theta_max         27.60
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    4.433
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5833
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2007)'
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plank
_exptl_crystal_F_000             1030
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.415
_refine_diff_density_min         -1.008
_refine_diff_density_rms         0.118
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.013(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         5139
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0299
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0334P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0656
_refine_ls_wR_factor_ref         0.0707
_reflns_number_gt                4242
_reflns_number_total             5139
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8b06090_si_001.cif
_cod_data_source_block           4728
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '_atom_site_symetry_multiplicity' was replaced with
'_atom_site_symmetry_multiplicity' as specified in the replacement
file
'/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/lists/replacement-tags.lst'.

Automatic conversion script
Id: cif_correct_tags 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21 21 2 '
_cod_database_code               4132760
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z'
'-x, -y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
U1 U 0.5000 0.5000 0.654620(17) 0.02390(7) Uani 1 2 d S
I1 I 0.5000 0.5000 0.39256(3) 0.04501(12) Uani 1 2 d S
P1 P 0.57438(11) 0.68893(8) 0.67920(12) 0.0268(3) Uani 1 1 d .
N1 N 0.3776(4) 0.5928(3) 0.7451(4) 0.0328(10) Uani 1 1 d .
C1 C 0.3614(4) 0.6836(3) 0.7487(5) 0.0308(12) Uani 1 1 d .
C2 C 0.2670(5) 0.7236(4) 0.7844(4) 0.0378(15) Uani 1 1 d .
H2 H 0.2115 0.6892 0.8128 0.050 Uiso 1 1 calc R
C3 C 0.2529(6) 0.8131(4) 0.7792(5) 0.0425(17) Uani 1 1 d .
H3 H 0.1871 0.8370 0.8002 0.057 Uiso 1 1 calc R
C4 C 0.3336(5) 0.8671(3) 0.7437(5) 0.0392(14) Uani 1 1 d .
C5 C 0.4295(5) 0.8288(3) 0.7115(4) 0.0331(13) Uani 1 1 d .
H5 H 0.4854 0.8645 0.6870 0.044 Uiso 1 1 calc R
C6 C 0.4459(5) 0.7404(3) 0.7142(4) 0.0308(12) Uani 1 1 d .
C7 C 0.3214(6) 0.9656(3) 0.7360(5) 0.0496(17) Uani 1 1 d .
H7a H 0.3523 0.9922 0.8026 0.074 Uiso 1 1 calc R
H7b H 0.2465 0.9803 0.7316 0.074 Uiso 1 1 calc R
H7c H 0.3575 0.9866 0.6688 0.074 Uiso 1 1 calc R
C8 C 0.6327(4) 0.7568(3) 0.5635(5) 0.0300(12) Uani 1 1 d .
H8 H 0.6414 0.8164 0.5925 0.040 Uiso 1 1 calc R
C9 C 0.5578(5) 0.7598(4) 0.4604(4) 0.0361(13) Uani 1 1 d .
H9a H 0.5908 0.7930 0.4003 0.054 Uiso 1 1 calc R
H9b H 0.4912 0.7867 0.4820 0.054 Uiso 1 1 calc R
H9c H 0.5444 0.7015 0.4340 0.054 Uiso 1 1 calc R
C10 C 0.7434(5) 0.7212(4) 0.5338(6) 0.0433(15) Uani 1 1 d .
H10a H 0.7364 0.6632 0.5038 0.065 Uiso 1 1 calc R
H10b H 0.7872 0.7199 0.6014 0.065 Uiso 1 1 calc R
H10c H 0.7765 0.7580 0.4774 0.065 Uiso 1 1 calc R
C11 C 0.6580(5) 0.7118(3) 0.8065(6) 0.0404(15) Uani 1 1 d .
H11 H 0.7237 0.6769 0.7998 0.054 Uiso 1 1 calc R
C12 C 0.5984(5) 0.6812(4) 0.9155(5) 0.0515(18) Uani 1 1 d .
H12a H 0.6457 0.6856 0.9801 0.077 Uiso 1 1 calc R
H12b H 0.5761 0.6217 0.9061 0.077 Uiso 1 1 calc R
H12c H 0.5365 0.7173 0.9278 0.077 Uiso 1 1 calc R
C13 C 0.6919(7) 0.8071(4) 0.8207(7) 0.074(3) Uani 1 1 d .
H13a H 0.6304 0.8442 0.8113 0.110 Uiso 1 1 calc R
H13b H 0.7449 0.8214 0.7642 0.110 Uiso 1 1 calc R
H13c H 0.7216 0.8154 0.8957 0.110 Uiso 1 1 calc R
C14 C 0.2885(5) 0.5395(3) 0.7808(5) 0.0361(14) Uani 1 1 d .
C15 C 0.2152(4) 0.5074(5) 0.7009(4) 0.0371(12) Uani 1 1 d .
C16 C 0.1326(5) 0.4521(3) 0.7376(6) 0.0468(16) Uani 1 1 d .
H16 H 0.0849 0.4298 0.6839 0.062 Uiso 1 1 calc R
C17 C 0.1198(5) 0.4295(4) 0.8508(6) 0.0485(17) Uani 1 1 d .
C18 C 0.1902(5) 0.4631(4) 0.9288(6) 0.0451(16) Uani 1 1 d .
H18 H 0.1813 0.4485 1.0054 0.060 Uiso 1 1 calc R
C19 C 0.2760(5) 0.5192(3) 0.8984(5) 0.0391(16) Uani 1 1 d .
C20 C 0.2225(6) 0.5310(4) 0.5757(6) 0.0481(16) Uani 1 1 d .
H20a H 0.2399 0.5917 0.5683 0.072 Uiso 1 1 calc R
H20b H 0.1548 0.5197 0.5393 0.072 Uiso 1 1 calc R
H20c H 0.2775 0.4966 0.5399 0.072 Uiso 1 1 calc R
C21 C 0.0313(5) 0.3685(4) 0.8886(6) 0.065(2) Uani 1 1 d .
H21a H -0.0354 0.3998 0.8918 0.098 Uiso 1 1 calc R
H21b H 0.0480 0.3457 0.9630 0.098 Uiso 1 1 calc R
H21c H 0.0252 0.3213 0.8350 0.098 Uiso 1 1 calc R
C22 C 0.3502(5) 0.5544(4) 0.9848(5) 0.0503(17) Uani 1 1 d .
H22a H 0.3280 0.5357 1.0595 0.075 Uiso 1 1 calc R
H22b H 0.3495 0.6170 0.9815 0.075 Uiso 1 1 calc R
H22c H 0.4216 0.5336 0.9698 0.075 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N1 U1 N1 126.2(2) 4_665 .
N1 U1 P1 65.04(11) 4_665 4_665
N1 U1 P1 109.69(11) . 4_665
N1 U1 P1 109.69(11) 4_665 .
N1 U1 P1 65.04(11) . .
P1 U1 P1 169.21(5) 4_665 .
N1 U1 I1 116.91(11) 4_665 .
N1 U1 I1 116.91(11) . .
P1 U1 I1 95.40(3) 4_665 .
P1 U1 I1 95.40(3) . .
C6 P1 C11 103.3(3) . .
C6 P1 C8 105.2(2) . .
C11 P1 C8 105.1(3) . .
C6 P1 U1 99.52(18) . .
C11 P1 U1 115.23(17) . .
C8 P1 U1 125.62(17) . .
C1 N1 C14 116.3(4) . .
C1 N1 U1 135.1(3) . .
C14 N1 U1 106.8(3) . .
C2 C1 N1 124.5(5) . .
C2 C1 C6 116.0(5) . .
N1 C1 C6 119.4(5) . .
C3 C2 C1 122.1(6) . .
C4 C3 C2 121.3(6) . .
C3 C4 C5 117.4(5) . .
C3 C4 C7 123.1(5) . .
C5 C4 C7 119.5(6) . .
C6 C5 C4 122.8(6) . .
C5 C6 C1 120.1(5) . .
C5 C6 P1 123.5(5) . .
C1 C6 P1 116.4(4) . .
C10 C8 C9 112.6(5) . .
C10 C8 P1 108.6(4) . .
C9 C8 P1 110.7(4) . .
C13 C11 C12 109.4(6) . .
C13 C11 P1 115.1(4) . .
C12 C11 P1 109.6(4) . .
C15 C14 C19 120.0(5) . .
C15 C14 N1 120.7(5) . .
C19 C14 N1 119.3(6) . .
C14 C15 C16 119.2(5) . .
C14 C15 C20 121.6(5) . .
C16 C15 C20 119.2(6) . .
C17 C16 C15 122.2(7) . .
C18 C17 C16 118.2(6) . .
C18 C17 C21 120.4(6) . .
C16 C17 C21 121.4(7) . .
C17 C18 C19 123.1(6) . .
C18 C19 C14 117.2(6) . .
C18 C19 C22 121.6(5) . .
C14 C19 C22 121.1(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 N1 2.337(4) 4_665
U1 N1 2.337(4) .
U1 P1 3.0542(12) 4_665
U1 P1 3.0542(12) .
U1 I1 3.0633(4) .
P1 C6 1.830(5) .
P1 C11 1.850(6) .
P1 C8 1.855(5) .
N1 C1 1.407(6) .
N1 C14 1.439(7) .
C1 C2 1.390(8) .
C1 C6 1.425(8) .
C2 C3 1.384(8) .
C3 C4 1.366(9) .
C4 C5 1.382(8) .
C4 C7 1.521(7) .
C5 C6 1.370(7) .
C8 C10 1.523(8) .
C8 C9 1.524(7) .
C11 C13 1.528(8) .
C11 C12 1.546(9) .
C14 C15 1.396(8) .
C14 C19 1.418(7) .
C15 C16 1.400(8) .
C15 C20 1.510(8) .
C16 C17 1.376(9) .
C17 C18 1.365(10) .
C17 C21 1.511(8) .
C18 C19 1.417(8) .
C19 C22 1.470(8) .
