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_7701665
_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         'C26 H46 N4 O6 P2 Ti'
_chemical_formula_sum            'C26 H44 N4 O6 P2 Ti'
_chemical_formula_weight         618.49
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-05-16
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   21.202(5)
_cell_length_b                   21.202(5)
_cell_length_c                   31.436(8)
_cell_measurement_reflns_used    9531
_cell_measurement_temperature    90.15
_cell_measurement_theta_max      30.615
_cell_measurement_theta_min      2.317
_cell_volume                     14131(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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      90.15
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_unetI/netI     0.0552
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            156780
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.046
_diffrn_reflns_theta_min         1.158
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.371
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6734
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_description       prism
_exptl_crystal_F_000             5248
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.18
_platon_squeeze_details          'TITL shelx I 41/a R = 0.07'
_refine_diff_density_max         0.690
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         156780
_refine_ls_number_restraints     426
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_gt           0.0517
_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/[\s^2^(Fo^2^)+(0.0515P)^2^+29.2744P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1227
_refine_ls_wR_factor_ref         0.1358
_reflns_Friedel_coverage         0.000
_reflns_number_gt                127717
_reflns_number_total             156780
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00911f2.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        14131(8)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7701665
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.936
_shelx_estimated_absorpt_t_min   0.872
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5060(12)
 0.4940(12)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C24A) = Uanis(C24)
4. 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
5. Others
 Sof(C1A)=Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=
 Sof(H5A)=Sof(C6A)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=1-FVAR(1)
 Sof(C1)=Sof(C2)=Sof(H2)=Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4)=Sof(C5)=Sof(H5)=
 Sof(C6)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=FVAR(1)
 Sof(H23C)=Sof(H23D)=Sof(C24A)=Sof(H24D)=Sof(H24E)=Sof(H24F)=1-FVAR(2)
 Sof(H23A)=Sof(H23B)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=FVAR(2)
 Fixed Sof: H26A(0.5) H26B(0.5) H26C(0.5) H26D(0.5) H26E(0.5) H26F(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C10(H10A,H10B), C23(H23A,H23B), C23(H23C,H23D), C25(H25A,H25B)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C2A(H2A), C3A(H3A), C4A(H4A), C5A(H5A),
 C0AA(H0AA), C18(H18), C19(H19), C20(H20)
6.c Fitted hexagon refined as free rotating group:
 C1(C2,C3,C4,C5,C6)
6.d Disordered Me refined with riding coordinates:
 C26(H26A,H26B,H26C,H26D,H26E,H26F)
6.e Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C7A(H7AA,H7AB,H7AC), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C),
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C24A(H24D,H24E,H24F)
;
_olex2_exptl_crystal_mounting_method cryo-loop
_olex2_submission_special_instructions 'No special instructions were received'