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_7701661
_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         'C24 H42 N4 O6 P2 Ti'
_chemical_formula_sum            'C24 H42 N4 O6 P2 Ti'
_chemical_formula_weight         592.45
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-11-01
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_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            4
_cell_length_a                   9.9388(2)
_cell_length_b                   15.5890(4)
_cell_length_c                   19.0437(5)
_cell_measurement_reflns_used    9970
_cell_measurement_temperature    90
_cell_measurement_theta_max      30.026
_cell_measurement_theta_min      2.312
_cell_volume                     2950.55(12)
_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
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  apex
_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  0.0343
_diffrn_reflns_av_unetI/netI     0.0527
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            20118
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.040
_diffrn_reflns_theta_min         2.139
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.441
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6748
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0549 before and 0.0493 after correction.
The Ratio of minimum to maximum transmission is 0.9046.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_description       prism
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.362
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details
;
 Flack x determined using 3004 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.008(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         8617
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0351
_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^)+(0.0333P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0726
_refine_ls_wR_factor_ref         0.0757
_reflns_Friedel_coverage         0.797
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                7621
_reflns_number_total             8617
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00911f2.cif
_cod_data_source_block           ls592-copy
_cod_database_code               7701661
_shelx_estimated_absorpt_t_max   0.929
_shelx_estimated_absorpt_t_min   0.879
_olex2_refinement_description
;
1. 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
2.a Secondary CH2 refined with riding coordinates:
 C00N(H00D,H00F), C00P(H00H,H00L), C00U(H00W,H00X), C00Z(H1AA,HF)
2.b Aromatic/amide H refined with riding coordinates:
 C00E(H00E), C00G(H00G), C00I(H00I), C00J(H00J), C00K(H00K), C00M(H00M),
 C00O(H00O), C00R(H00R), C00S(H00S), C00X(H00)
2.c Idealised Me refined as rotating group:
 C00L(H00A,H00B,H00C), C00Q(H00N,H00P,H00Q), C00T(H00T,H00U,H00V), C00V(H00Y,H,
 HA), C00W(H00Z,HB,HC), C00Y(H0AA,HD,HE), C010(H01A,H01B,H01C), C011(H01D,H01E,
 H01F)
;
_shelx_res_checksum              11036
_shelx_shelxl_version_number     2014/7
_olex2_submission_original_sample_id mp-302
_olex2_submission_special_instructions 'No special instructions were received'