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#$Date: 2023-07-05 11:45:30 +0300 (Wed, 05 Jul 2023) $
#$Revision: 284833 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/92/1569256.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_1569256
loop_
_publ_author_name
'Jin, Li'
'Zhang, Guoqiang'
'Yang, Xiaoqin'
'Song, Jinyi'
'Wang, Jin'
'Liao, Qian'
_publ_section_title
;
 A synthetic cycle for iminophosphorane synthesis involving direct
 intermolecular NP bond formation on N₂-derived
 molybdenum nitride.
;
_journal_issue                   51
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              7955
_journal_page_last               7958
_journal_paper_doi               10.1039/d3cc01925j
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         C8H13PN,I
_chemical_formula_sum            'C8 H13 I N P'
_chemical_formula_weight         281.06
_chemical_properties_physical    Moisture-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2023-04-11 deposited with the CCDC.	2023-05-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.818(7)
_cell_length_b                   6.851(3)
_cell_length_c                   12.453(5)
_cell_measurement_reflns_used    1690
_cell_measurement_temperature    274(2)
_cell_measurement_theta_max      24.16
_cell_measurement_theta_min      3.17
_cell_volume                     1093.6(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      274(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0658
_diffrn_reflns_av_unetI/netI     0.0494
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4626
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        24.468
_diffrn_reflns_theta_max         24.468
_diffrn_reflns_theta_min         3.179
_exptl_absorpt_coefficient_mu    3.021
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.5304
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.707
_exptl_crystal_description       needle
_exptl_crystal_F_000             544
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene'
_exptl_crystal_size_max          0.656
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.087
_refine_diff_density_max         0.919
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     69
_refine_ls_number_reflns         966
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0349
_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/[σ²(Fo²)+(0.0421P)²+0.5684P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0843
_refine_ls_wR_factor_ref         0.0907
_reflns_Friedel_coverage         0.000
_reflns_number_gt                816
_reflns_number_total             966
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3cc01925j2.cif
_cod_data_source_block           H2NPMe2PhI
_cod_depositor_comments
'Adding full bibliography for 1569251--1569256.cif.'
_cod_database_code               1569256
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;
_shelx_estimated_absorpt_t_min   0.242
_shelx_estimated_absorpt_t_max   0.779
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.33630(3) 0.7500 0.83823(4) 0.0586(3) Uani 1 2 d S T P . .
P1 P 0.55740(14) 0.2500 0.81443(13) 0.0477(4) Uani 1 2 d S T P . .
N1 N 0.4477(5) 0.2500 0.8809(5) 0.0632(16) Uani 1 2 d DS T P . .
H1A H 0.410(5) 0.135(7) 0.876(5) 0.09(2) Uiso 1 1 d D . . . .
C1 C 0.5416(6) 0.2500 0.6729(5) 0.0488(15) Uani 1 2 d S T P . .
C2 C 0.4429(6) 0.2500 0.6270(6) 0.0663(19) Uani 1 2 d S T P . .
H2 H 0.3838 0.2500 0.6704 0.080 Uiso 1 2 calc R U P . .
C7 C 0.6250(5) 0.4636(8) 0.8527(4) 0.0682(14) Uani 1 1 d . . . . .
H7A H 0.5802 0.5747 0.8441 0.102 Uiso 1 1 calc R U . . .
H7B H 0.6857 0.4790 0.8083 0.102 Uiso 1 1 calc R U . . .
H7C H 0.6459 0.4531 0.9265 0.102 Uiso 1 1 calc R U . . .
C6 C 0.6277(6) 0.2500 0.6056(7) 0.068(2) Uani 1 2 d S T P . .
H6 H 0.6949 0.2500 0.6338 0.081 Uiso 1 2 calc R U P . .
C3 C 0.4330(8) 0.2500 0.5180(7) 0.079(2) Uani 1 2 d S T P . .
H3 H 0.3668 0.2500 0.4875 0.094 Uiso 1 2 calc R U P . .
C5 C 0.6120(9) 0.2500 0.4961(6) 0.082(2) Uani 1 2 d S T P . .
H5 H 0.6694 0.2500 0.4504 0.098 Uiso 1 2 calc R U P . .
C4 C 0.5169(9) 0.2500 0.4543(6) 0.081(3) Uani 1 2 d S T P . .
H4 H 0.5084 0.2500 0.3802 0.098 Uiso 1 2 calc R U P . .
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'
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
_geom_angle_publ_flag
N1 P1 C7 106.6(2) . 7_565 ?
N1 P1 C7 106.6(2) . . ?
C7 P1 C7 111.9(4) 7_565 . ?
N1 P1 C1 114.0(3) . . ?
C7 P1 C1 108.9(2) 7_565 . ?
C7 P1 C1 108.9(2) . . ?
P1 N1 H1A 114(4) . . ?
C6 C1 C2 118.5(7) . . ?
C6 C1 P1 120.7(6) . . ?
C2 C1 P1 120.8(6) . . ?
C3 C2 C1 119.6(8) . . ?
C3 C2 H2 120.2 . . ?
C1 C2 H2 120.2 . . ?
P1 C7 H7A 109.5 . . ?
P1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
P1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C6 C1 118.8(8) . . ?
C5 C6 H6 120.6 . . ?
C1 C6 H6 120.6 . . ?
C4 C3 C2 121.1(8) . . ?
C4 C3 H3 119.5 . . ?
C2 C3 H3 119.5 . . ?
C4 C5 C6 121.5(9) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 H5 119.3 . . ?
C5 C4 C3 120.5(8) . . ?
C5 C4 H4 119.7 . . ?
C3 C4 H4 119.7 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 N1 1.631(6) . ?
P1 C7 1.766(5) 7_565 ?
P1 C7 1.766(5) . ?
P1 C1 1.774(6) . ?
N1 H1A 0.92(4) . ?
C1 C6 1.385(10) . ?
C1 C2 1.389(10) . ?
C2 C3 1.363(10) . ?
C2 H2 0.9300 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C6 C5 1.379(11) . ?
C6 H6 0.9300 . ?
C3 C4 1.336(12) . ?
C3 H3 0.9300 . ?
C5 C4 1.326(12) . ?
C5 H5 0.9300 . ?
C4 H4 0.9300 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 P1 C1 C6 180.000(1) . . . . ?
C7 P1 C1 C6 -61.1(2) 7_565 . . . ?
C7 P1 C1 C6 61.1(2) . . . . ?
N1 P1 C1 C2 0.000(1) . . . . ?
C7 P1 C1 C2 118.9(2) 7_565 . . . ?
C7 P1 C1 C2 -118.9(2) . . . . ?
C6 C1 C2 C3 0.000(2) . . . . ?
P1 C1 C2 C3 180.000(1) . . . . ?
C2 C1 C6 C5 0.000(2) . . . . ?
P1 C1 C6 C5 180.000(1) . . . . ?
C1 C2 C3 C4 0.000(2) . . . . ?
C1 C6 C5 C4 0.000(2) . . . . ?
C6 C5 C4 C3 0.000(2) . . . . ?
C2 C3 C4 C5 0.000(2) . . . . ?
