Mono, bis, and tris(phosphoramidate) titanium complexes: synthesis, structure, and reactivity investigations.
Perry, Mitchell R.; Gilmour, Damon J.; Schafer, Laurel L.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 9782–9790; doi:10.1039/c9dt00911f

data_7701662
_publ_section_title
;
 Mono, bis, and tris(phosphoramidate) titanium complexes: synthesis,
 structure, and reactivity investigations.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9782
_journal_page_last               9790
_journal_paper_doi               10.1039/c9dt00911f
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C28 H50 N4 O6 P2 Ti'
_chemical_formula_sum            'C28 H50 N4 O6 P2 Ti'
_chemical_formula_weight         648.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-06-07
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2019-03-25 deposited with the CCDC.	2019-04-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.550(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.113(3)
_cell_length_b                   10.978(2)
_cell_length_c                   11.644(2)
_cell_measurement_reflns_used    5575
_cell_measurement_temperature    90
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      2.68
_cell_volume                     1666.1(6)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      90
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker-Nonius APEXII CCD area detector'
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9380
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.394
_diffrn_reflns_theta_max         25.394
_diffrn_reflns_theta_min         1.894
_exptl_absorpt_coefficient_mu    0.397
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6493
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0561 before and 0.0455 after correction. The Ratio of minimum to maximum transmission is 0.8713. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_description       prism
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.252
_exptl_crystal_size_mid          0.133
_exptl_crystal_size_min          0.103
_refine_diff_density_max         0.604
_refine_diff_density_min         -1.124
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.14(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         2916
_refine_ls_number_restraints     592
_refine_ls_restrained_S_all      0.932
_refine_ls_R_factor_all          0.0815
_refine_ls_R_factor_gt           0.0757
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+20.2496P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1576
_refine_ls_wR_factor_ref         0.1608
_reflns_Friedel_coverage         0.898
_reflns_Friedel_fraction_full    0.981
_reflns_Friedel_fraction_max     0.981
_reflns_number_gt                2706
_reflns_number_total             2916
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00911f2.cif
_cod_data_source_block           ls627_1
_cod_original_cell_volume        1666.2(6)
_cod_database_code               7701662
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.960
_shelx_estimated_absorpt_t_min   0.907
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.86(11)
 0.14(11)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C9-C10
 1.4 with sigma of 0.02
 C9-C10 \\sim C12-C11 \\sim C9A-C10A \\sim C12A-C11A
 with sigma of 0.01
 O2A-C11A \\sim O1A-C9A \\sim O2-C11 \\sim O1-C9
 with sigma of 0.01
 N2-C13 \\sim N2-C14 \\sim N2A-C13A \\sim N2A-C14A
 with sigma of 0.01
 P1-O2 \\sim P1-O1 \\sim P1A-O1A \\sim P1A-O2A
 with sigma of 0.01
 P1A-O3A \\sim P1-O3
 with sigma of 0.01
 P1A-N1A \\sim P1-N1
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(C9A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O3) = Uanis(O3A)
Uanis(C1A) = Uanis(C1)
Uanis(C8) = Uanis(C8A)
Uanis(C2) = Uanis(C2A)
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C1A)=Sof(C2A)=Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=Sof(H5A)=
 Sof(C6A)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=
 Sof(H8AC)=Sof(P1A)=Sof(C10A)=Sof(H10D)=Sof(H10E)=Sof(H10F)=Sof(C9A)=Sof(H9AA)=
 Sof(H9AB)=Sof(O1A)=Sof(C11A)=Sof(H11C)=Sof(H11D)=Sof(O2A)=Sof(C12A)=Sof(H12D)=
 Sof(H12E)=Sof(H12F)=Sof(N1A)=Sof(O3A)=1-FVAR(1)
 Sof(P1)=Sof(O1)=Sof(O2)=Sof(O3)=Sof(N1)=Sof(C1)=Sof(C2)=Sof(C3)=Sof(H3)=
 Sof(C4)=Sof(H4)=Sof(C5)=Sof(H5)=Sof(C6)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=
 Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(C10)=
 Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(C12)=Sof(H12A)=
 Sof(H12B)=Sof(H12C)=FVAR(1)
 Fixed Sof: N2(0.5) C13(0.5) H13A(0.5) H13B(0.5) H13C(0.5) C14(0.5) H14A(0.5)
 H14B(0.5) H14C(0.5) N2A(0.5) C14A(0.5) H14D(0.5) H14E(0.5) H14F(0.5) C13A(0.5)
 H13D(0.5) H13E(0.5) H13F(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C11(H11A,H11B), C9A(H9AA,H9AB), C11A(H11C,H11D)
7.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C3A(H3A), C4A(H4A), C5A(H5A)
7.c Fitted hexagon refined as free rotating group:
 C1(C2,C3,C4,C5,C6), C1A(C2A,C3A,C4A,C5A,C6A)
7.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C7A(H7AA,H7AB,H7AC), C8A(H8AA,H8AB,
 H8AC), C10A(H10D,H10E,H10F), C12A(H12D,H12E,H12F), C14A(H14D,H14E,H14F),
 C13A(H13D,H13E,H13F)
;
_olex2_exptl_crystal_mounting_method goniometer
_olex2_submission_original_sample_id vc-7
_olex2_submission_special_instructions 'No special instructions were received'