#------------------------------------------------------------------------------
#$Date: 2023-12-12 00:20:26 +0200 (Tue, 12 Dec 2023) $
#$Revision: 288221 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/54/41/1544184.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_1544184
loop_
_publ_author_name
'Grant, Lauren N.'
'Pinter, Balazs'
'Kurogi, Takashi'
'Carroll, Maria E.'
'Wu, Gang'
'Manor, Brian C.'
'Carroll, Patrick J.'
'Mindiola, Daniel J.'
_publ_section_title
;
 Molecular titanium nitrides: nucleophiles unleashed.
;
_journal_issue                   2
_journal_name_full               'Chemical science'
_journal_page_first              1209
_journal_page_last               1224
_journal_paper_doi               10.1039/c6sc03422e
_journal_volume                  8
_journal_year                    2017
_chemical_formula_moiety         '2(C50 H76 N3 P3 Ti), 2(C5 H12)'
_chemical_formula_sum            'C110 H176 N6 P6 Ti2'
_chemical_formula_weight         1864.18
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-06-22
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-07-04 deposited with the CCDC.
2016-09-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.499(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.5929(8)
_cell_length_b                   12.9042(5)
_cell_length_c                   22.7421(14)
_cell_measurement_reflns_used    9815
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.22
_cell_volume                     5396.5(5)
_computing_data_collection       'Bruker APEX2 v2014.11-0'
_computing_data_reduction        'Bruker SAINT v8.34A'
_computing_molecular_graphics    'Mercury v3.6'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device       'CCD area detector'
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            84659
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.590
_diffrn_reflns_theta_min         1.811
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.284
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6334
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2014/4'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.147
_exptl_crystal_description       prism
_exptl_crystal_F_000             2024
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.262
_refine_diff_density_min         -1.056
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         6146
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0748
_refine_ls_R_factor_gt           0.0662
_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)+(0.1013P)²+16.4956P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1786
_refine_ls_wR_factor_ref         0.1890
_reflns_number_gt                5325
_reflns_number_total             6146
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6sc03422e2.cif
_cod_data_source_block           9152
_cod_depositor_comments
;Adding full bibliography for 1544183--1544188.cif.

 Adding full bibliography for 1544183--1544188.cif.

The following automatic conversions were performed:

data name '_exptl_crystal_color' was replaced with
'_exptl_crystal_colour' as specified in the replacement file
'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_database_code               1544184
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -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
Ti1 Ti 0.2500 0.24079(4) 0.5000 0.01619(16) Uani 1 2 d S T P . .
P1 P 0.10610(3) 0.25694(4) 0.45990(3) 0.01867(16) Uani 1 1 d . . . . .
P2 P 0.26882(8) -0.02285(11) 0.51988(7) 0.0344(3) Uani 0.5 1 d . . . . .
N1 N 0.20758(9) 0.30854(14) 0.56988(8) 0.0173(4) Uani 1 1 d . . . . .
N2 N 0.2500 0.1049(2) 0.5000 0.0280(6) Uani 1 2 d S T P A .
C1 C 0.13539(11) 0.29916(17) 0.58000(10) 0.0191(4) Uani 1 1 d . . . . .
C2 C 0.11349(13) 0.32258(19) 0.63524(10) 0.0246(5) Uani 1 1 d . . . . .
H2 H 0.1472 0.3498 0.6656 0.033 Uiso 1 1 calc R . . . .
C3 C 0.04241(14) 0.3057(2) 0.64508(11) 0.0287(5) Uani 1 1 d . . . . .
H3 H 0.0297 0.3221 0.6820 0.038 Uiso 1 1 calc R . . . .
C4 C -0.01018(13) 0.26518(19) 0.60167(12) 0.0280(5) Uani 1 1 d . . . . .
C5 C 0.00988(13) 0.24734(18) 0.54617(12) 0.0246(5) Uani 1 1 d . . . . .
H5 H -0.0249 0.2226 0.5158 0.033 Uiso 1 1 calc R . . . .
C6 C 0.08050(12) 0.26520(17) 0.53408(10) 0.0197(4) Uani 1 1 d . . . . .
C7 C -0.08644(16) 0.2437(2) 0.61365(15) 0.0395(7) Uani 1 1 d . . . . .
H7a H -0.1192 0.2933 0.5928 0.059 Uiso 1 1 calc GR . . . .
H7b H -0.0880 0.2489 0.6555 0.059 Uiso 1 1 calc GR . . . .
H7c H -0.1006 0.1751 0.6002 0.059 Uiso 1 1 calc GR . . . .
C8 C 0.04496(15) 0.1574(2) 0.42090(13) 0.0372(6) Uani 1 1 d . . . . .
H8 H -0.0045 0.1754 0.4273 0.049 Uiso 1 1 calc R . . . .
C9 C 0.0596(3) 0.0514(3) 0.4451(2) 0.0685(12) Uani 1 1 d . . . . .
H9a H 0.0204 0.0062 0.4293 0.103 Uiso 1 1 calc GR . . . .
H9b H 0.0635 0.0532 0.4877 0.103 Uiso 1 1 calc GR . . . .
H9c H 0.1043 0.0262 0.4341 0.103 Uiso 1 1 calc GR . . . .
C10 C 0.04479(17) 0.1570(3) 0.35310(14) 0.0477(8) Uani 1 1 d . . . . .
H10a H 0.0910 0.1329 0.3446 0.072 Uiso 1 1 calc GR . . . .
H10b H 0.0362 0.2259 0.3378 0.072 Uiso 1 1 calc GR . . . .
H10c H 0.0071 0.1118 0.3346 0.072 Uiso 1 1 calc GR . . . .
C11 C 0.06678(13) 0.3777(2) 0.42312(10) 0.0262(5) Uani 1 1 d . . . . .
H11 H 0.0835 0.3820 0.3843 0.035 Uiso 1 1 calc R . . . .
C12 C 0.09745(16) 0.4715(2) 0.45912(12) 0.0319(6) Uani 1 1 d . . . . .
H12a H 0.0814 0.5338 0.4381 0.048 Uiso 1 1 calc GR . . . .
H12b H 0.1496 0.4687 0.4649 0.048 Uiso 1 1 calc GR . . . .
H12c H 0.0807 0.4711 0.4971 0.048 Uiso 1 1 calc GR . . . .
C13 C -0.01630(15) 0.3842(3) 0.41206(14) 0.0399(7) Uani 1 1 d . . . . .
H13a H -0.0348 0.3769 0.4491 0.060 Uiso 1 1 calc GR . . . .
H13b H -0.0354 0.3298 0.3855 0.060 Uiso 1 1 calc GR . . . .
H13c H -0.0309 0.4501 0.3947 0.060 Uiso 1 1 calc GR . . . .
C14 C 0.25625(11) 0.34618(17) 0.62070(9) 0.0185(4) Uani 1 1 d . . . . .
C15 C 0.28818(12) 0.27609(19) 0.66451(10) 0.0221(4) Uani 1 1 d . . . . .
C16 C 0.33678(13) 0.3135(2) 0.71251(10) 0.0272(5) Uani 1 1 d . . . . .
H16 H 0.3583 0.2671 0.7411 0.036 Uiso 1 1 calc R . . . .
C17 C 0.35385(13) 0.4181(2) 0.71870(10) 0.0291(5) Uani 1 1 d . . . . .
C18 C 0.31879(14) 0.4866(2) 0.67704(11) 0.0274(5) Uani 1 1 d . . . . .
H18 H 0.3284 0.5571 0.6815 0.036 Uiso 1 1 calc R . . . .
C19 C 0.26946(12) 0.45268(18) 0.62848(10) 0.0220(4) Uani 1 1 d . . . . .
C20 C 0.26724(14) 0.16361(19) 0.66156(11) 0.0270(5) Uani 1 1 d . . . . .
H20a H 0.2924 0.1281 0.6956 0.040 Uiso 1 1 calc GR . . . .
H20b H 0.2802 0.1335 0.6260 0.040 Uiso 1 1 calc GR . . . .
H20c H 0.2157 0.1574 0.6612 0.040 Uiso 1 1 calc GR . . . .
C21 C 0.40940(17) 0.4563(3) 0.76950(13) 0.0420(7) Uani 1 1 d . . . . .
H21a H 0.4570 0.4538 0.7580 0.063 Uiso 1 1 calc GR . . . .
H21b H 0.4082 0.4130 0.8037 0.063 Uiso 1 1 calc GR . . . .
H21c H 0.3982 0.5264 0.7791 0.063 Uiso 1 1 calc GR . . . .
C22 C 0.22853(15) 0.53135(19) 0.58755(11) 0.0293(5) Uani 1 1 d . . . . .
H22a H 0.1776 0.5268 0.5902 0.044 Uiso 1 1 calc GR . . . .
H22b H 0.2361 0.5178 0.5474 0.044 Uiso 1 1 calc GR . . . .
H22c H 0.2458 0.5996 0.5989 0.044 Uiso 1 1 calc GR . . . .
C23 C 0.1838(4) -0.0858(4) 0.5370(3) 0.0426(14) Uani 0.5 1 d D . . A 1
H23 H 0.1475 -0.0911 0.5012 0.057 Uiso 0.5 1 calc R . . A 1
C23' C 0.2235(4) -0.0732(4) 0.5568(3) 0.0432(14) Uani 0.5 1 d D . . A 2
H23' H 0.2684 -0.0572 0.5836 0.057 Uiso 0.5 1 calc R . . A 2
C24 C 0.15654(19) -0.0226(3) 0.58245(17) 0.0531(8) Uani 1 1 d D . . . .
H24a H 0.1420 0.0441 0.5661 0.080 Uiso 0.5 1 calc R . . A 1
H24b H 0.1155 -0.0565 0.5952 0.080 Uiso 0.5 1 calc R . . A 1
H24c H 0.1942 -0.0141 0.6158 0.080 Uiso 0.5 1 calc R . . A 1
H24x H 0.1611 0.0515 0.5823 0.080 Uiso 0.5 1 calc R . . A 2
H24y H 0.1120 -0.0425 0.5581 0.080 Uiso 0.5 1 calc R . . A 2
H24z H 0.1560 -0.0463 0.6224 0.080 Uiso 0.5 1 calc R . . A 2
C25 C 0.2076(2) -0.1921(3) 0.5601(2) 0.0670(11) Uani 1 1 d D . . . .
H25a H 0.2251 -0.2311 0.5292 0.100 Uiso 0.5 1 calc R . . A 1
H25b H 0.2458 -0.1852 0.5933 0.100 Uiso 0.5 1 calc R . . A 1
H25c H 0.1671 -0.2276 0.5727 0.100 Uiso 0.5 1 calc R . . A 1
H25x H 0.2455 -0.2303 0.5454 0.100 Uiso 0.5 1 calc R . . A 2
H25y H 0.2058 -0.2114 0.6007 0.100 Uiso 0.5 1 calc R . . A 2
H25z H 0.1618 -0.2075 0.5363 0.100 Uiso 0.5 1 calc R . . A 2
C26 C 0.1418(5) 0.6063(10) 0.7430(5) 0.114(5) Uani 0.5 1 d . U . B -1
H26a H 0.1310 0.5425 0.7616 0.171 Uiso 0.5 1 calc R . . B -1
H26b H 0.1050 0.6567 0.7476 0.171 Uiso 0.5 1 calc R . . B -1
H26c H 0.1428 0.5945 0.7015 0.171 Uiso 0.5 1 calc R . . B -1
C27 C 0.2159(4) 0.6466(7) 0.7723(3) 0.096(3) Uani 0.5 1 d G U . B -1
H27a H 0.2526 0.5946 0.7683 0.128 Uiso 0.5 1 calc R . . B -1
H27b H 0.2147 0.6567 0.8144 0.128 Uiso 0.5 1 calc R . . B -1
C28 C 0.2380(5) 0.7487(8) 0.7455(5) 0.102(4) Uani 0.5 1 d G U . B -1
H28a H 0.2391 0.7385 0.7033 0.136 Uiso 0.5 1 calc R . . B -1
H28b H 0.2012 0.8006 0.7494 0.136 Uiso 0.5 1 calc R . . B -1
C29 C 0.3122(4) 0.7900(7) 0.7744(3) 0.105(4) Uani 0.5 1 d G U . B -1
H29a H 0.3112 0.8004 0.8165 0.139 Uiso 0.5 1 calc R . . B -1
H29b H 0.3490 0.7383 0.7704 0.139 Uiso 0.5 1 calc R . . B -1
C30 C 0.3335(6) 0.8919(8) 0.7471(6) 0.125(6) Uani 0.5 1 d G U . B -1
H30a H 0.3802 0.9138 0.7670 0.187 Uiso 0.5 1 calc R . . B -1
H30b H 0.3358 0.8819 0.7056 0.187 Uiso 0.5 1 calc R . . B -1
H30c H 0.2979 0.9440 0.7518 0.187 Uiso 0.5 1 calc R . . B -1
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'
Ti Ti 0.2776 0.4457 '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
P1 Ti1 P1 171.16(3) 2_556 .
N1 Ti1 P1 75.88(5) 2_556 2_556
N1 Ti1 P1 100.30(5) 2_556 .
N1 Ti1 P1 75.88(5) . .
N1 Ti1 P1 100.30(5) . 2_556
N1 Ti1 N1 130.02(10) 2_556 .
N2 Ti1 P1 94.419(17) . .
N2 Ti1 P1 94.420(17) . 2_556
N2 Ti1 N1 114.99(5) . .
N2 Ti1 N1 114.99(5) . 2_556
C6 P1 Ti1 94.19(7) . .
C6 P1 C8 104.96(12) . .
C6 P1 C11 103.15(10) . .
C8 P1 Ti1 127.94(10) . .
C8 P1 C11 101.08(13) . .
C11 P1 Ti1 121.21(8) . .
N2 P2 C23 108.90(19) . .
N2 P2 C23' 97.3(2) . 2_556
C1 N1 Ti1 124.96(14) . .
C1 N1 C14 113.61(17) . .
C14 N1 Ti1 119.49(13) . .
P2 N2 Ti1 162.21(6) . .
P2 N2 Ti1 162.21(6) 2_556 .
P2 N2 P2 35.59(12) 2_556 .
N1 C1 C2 122.6(2) . .
N1 C1 C6 120.60(19) . .
C2 C1 C6 116.8(2) . .
C3 C2 C1 121.1(2) . .
C4 C3 C2 122.2(2) . .
C3 C4 C5 117.0(2) . .
C3 C4 C7 121.6(3) . .
C5 C4 C7 121.3(3) . .
C4 C5 C6 122.5(2) . .
C1 C6 P1 116.23(16) . .
C5 C6 P1 123.58(18) . .
C5 C6 C1 120.0(2) . .
C9 C8 P1 113.3(2) . .
C9 C8 C10 109.9(3) . .
C10 C8 P1 113.1(2) . .
C12 C11 P1 109.36(16) . .
C12 C11 C13 109.5(2) . .
C13 C11 P1 116.02(19) . .
C15 C14 N1 119.9(2) . .
C19 C14 N1 120.54(19) . .
C19 C14 C15 119.5(2) . .
C14 C15 C20 120.6(2) . .
C16 C15 C14 119.1(2) . .
C16 C15 C20 120.2(2) . .
C17 C16 C15 121.8(2) . .
C16 C17 C21 120.9(2) . .
C18 C17 C16 118.2(2) . .
C18 C17 C21 120.8(3) . .
C17 C18 C19 121.9(2) . .
C14 C19 C22 121.3(2) . .
C18 C19 C14 119.2(2) . .
C18 C19 C22 119.4(2) . .
C24 C23 P2 107.2(4) . .
C24 C23 C25 111.9(5) . .
C25 C23 P2 104.7(4) . .
C24 C23' P2 111.6(4) . 2_556
C25 C23' P2 115.0(4) . 2_556
C25 C23' C24 102.8(4) . .
C26 C27 C28 113.3 . .
C29 C28 C27 113.8 . .
C30 C29 C28 113.3 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ti1 P1 2.7040(6) 2_556
Ti1 P1 2.7041(6) .
Ti1 N1 2.0695(18) .
Ti1 N1 2.0695(18) 2_556
Ti1 N2 1.753(3) .
P1 C6 1.822(2) .
P1 C8 1.852(3) .
P1 C11 1.866(2) .
P2 N2 1.732(3) .
P2 C23 1.868(7) .
P2 C23' 1.887(7) 2_556
N1 C1 1.400(3) .
N1 C14 1.443(3) .
N2 P2 1.732(3) 2_556
C1 C2 1.410(3) .
C1 C6 1.417(3) .
C2 C3 1.390(3) .
C3 C4 1.385(4) .
C4 C5 1.387(4) .
C4 C7 1.509(3) .
C5 C6 1.400(3) .
C8 C9 1.485(5) .
C8 C10 1.541(4) .
C11 C12 1.524(4) .
C11 C13 1.530(3) .
C14 C15 1.410(3) .
C14 C19 1.403(3) .
C15 C16 1.396(3) .
C15 C20 1.502(3) .
C16 C17 1.388(4) .
C17 C18 1.386(4) .
C17 C21 1.514(3) .
C18 C19 1.397(3) .
C19 C22 1.506(3) .
C23 C24 1.466(6) .
C23 C25 1.512(6) .
C23' P2 1.887(7) 2_556
C23' C24 1.591(6) .
C23' C25 1.566(6) .
C26 C27 1.5310 .
C27 C28 1.5331 .
C28 C29 1.5331 .
C29 C30 1.5310 .
