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_7701663
_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         'C36 H66 N4 O6 P2 Ti, 0.5[C7H8]'
_chemical_formula_sum            'C39.5 H70 N4 O6 P2 Ti'
_chemical_formula_weight         806.86
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-09-01
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2019-03-25 deposited with the CCDC.	2019-04-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.962(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7429(10)
_cell_length_b                   22.594(2)
_cell_length_c                   16.9276(14)
_cell_measurement_reflns_used    9960
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.82
_cell_measurement_theta_min      2.16
_cell_volume                     4485.2(7)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker Apex-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0816
_diffrn_reflns_av_unetI/netI     0.0776
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            58172
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.597
_diffrn_reflns_theta_min         1.504
_exptl_absorpt_coefficient_mu    0.304
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6499
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0819 before and 0.0639 after correction. The Ratio of minimum to maximum transmission is 0.8720. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.116
_exptl_crystal_description       prism
_exptl_crystal_F_000             1612
_exptl_crystal_size_max          0.357
_exptl_crystal_size_mid          0.257
_exptl_crystal_size_min          0.207
_refine_diff_density_max         0.292
_refine_diff_density_min         -0.360
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         8365
_refine_ls_number_restraints     745
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.0867
_refine_ls_R_factor_gt           0.0453
_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^)+(0.0360P)^2^+2.0292P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0891
_refine_ls_wR_factor_ref         0.1005
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5534
_reflns_number_total             8365
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00911f2.cif
_cod_data_source_block           ls558_sq
_cod_original_formula_sum        'C39.50 H70 N4 O6 P2 Ti'
_cod_database_code               7701663
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.940
_shelx_estimated_absorpt_t_min   0.899
_olex2_refinement_description
;
1. 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
2. Restrained distances
 C01E-C010 \\sim C01F-C010
 with sigma of 0.01
3. 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
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(H01C)=Sof(H01D)=Sof(C01F)=Sof(H3AA)=Sof(HM)=Sof(HN)=1-FVAR(1)
 Sof(H01A)=Sof(H01B)=Sof(C01E)=Sof(H2AA)=Sof(HK)=Sof(HL)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C00M(H00M), C00N(H00N), C00U(H00U), C00W(H00W)
6.b Secondary CH2 refined with riding coordinates:
 C00J(H00A,H00B), C00Q(H00C,H00D), C010(H01A,H01B), C010(H01C,H01D), C015(H01Q,
 H01R)
6.c Aromatic/amide H refined with riding coordinates:
 C00L(H00L), C00O(H00O), C00P(H00P), C00S(H00S), C00T(H00T), C00X(H00X)
6.d Idealised Me refined as rotating group:
 C00R(H00E,H00F,H00G), C00V(H00H,H00I,H00J), C00Y(H00K,H00Q,H00R), C00Z(H00V,
 H00Y,H), C011(H01E,H01F,H01G), C012(H01H,H01I,H01J), C013(H01K,H01L,H01M),
 C014(H01N,H01O,H01P), C016(H01S,H01T,H01U), C017(H01V,H01W,H01X), C018(H01Y,HA,
 HB), C019(H01Z,HC,HD), C01A(H01,HE,HF), C01B(H0AA,HG,HH), C01D(H1AA,HI,HJ),
 C01E(H2AA,HK,HL), C01F(H3AA,HM,HN)
;
_shelx_res_checksum              54250
_shelx_fab_checksum              31138
_olex2_submission_special_instructions 'No special instructions were received'