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_7701664
_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         'C38 H63 N4 O9 P3 Ti'
_chemical_formula_sum            'C38 H63 N4 O9 P3 Ti'
_chemical_formula_weight         860.73
_chemical_name_systematic        mp-218
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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                 94.609(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2852(7)
_cell_length_b                   17.6497(9)
_cell_length_c                   20.5001(12)
_cell_measurement_reflns_used    8082
_cell_measurement_temperature    100
_cell_measurement_theta_max      24.984
_cell_measurement_theta_min      2.196
_cell_volume                     4430.7(4)
_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      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Apex-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0732
_diffrn_reflns_av_unetI/netI     0.0608
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            45257
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.427
_diffrn_reflns_theta_min         1.525
_exptl_absorpt_coefficient_mu    0.355
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5847
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0880 before and 0.0696 after correction. The Ratio of minimum to maximum transmission is 0.7845. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_description       prism
_exptl_crystal_F_000             1832
_exptl_crystal_size_max          0.218
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.047
_refine_diff_density_max         0.684
_refine_diff_density_min         -0.550
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     510
_refine_ls_number_reflns         8153
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0455
_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^)+(0.0513P)^2^+3.0537P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1035
_refine_ls_wR_factor_ref         0.1190
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5970
_reflns_number_total             8153
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00911f2.cif
_cod_data_source_block           mo_ls609_0m
_cod_database_code               7701664
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.983
_shelx_estimated_absorpt_t_min   0.927
_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:
 C00L(H00A,H00B), C00Q(H00C,H00D), C012(H01D,H01E), C015(H01I,H01J), C01A(H01W,
 H01X), C01I(H4AA,HJ)
2.b Aromatic/amide H refined with riding coordinates:
 C00N(H00N), C00O(H00O), C00R(H00R), C00X(H00X), C00Z(H00Z), C011(H011),
 C013(H013), C01C(H01Z), C01D(H01)
2.c Idealised Me refined as rotating group:
 C00T(H00E,H00F,H00G), C00V(H00H,H00I,H00J), C010(H01A,H01B,H01C), C014(H01F,
 H01G,H01H), C016(H01K,H01L,H01M), C017(H01N,H01O,H01P), C018(H01Q,H01R,H01S),
 C019(H01T,H01U,H01V), C01B(H01Y,H,HA), C01E(H0AA,HB,HC), C01F(H1AA,HD,HE),
 C01G(H2AA,HF,HG), C01H(H3AA,HH,HI), C01J(H5AA,HK,HL)
;
_olex2_exptl_crystal_mounting_method 'Cryo loop'
_olex2_submission_original_sample_id mp-218
_olex2_submission_special_instructions 'No special instructions were received'