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_7701660
_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         '4(C18 H37 N4 O3 P Ti)'
_chemical_formula_sum            'C72 H148 N16 O12 P4 Ti4'
_chemical_formula_weight         1745.54
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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                91.59
_cell_angle_beta                 91.82
_cell_angle_gamma                90.66
_cell_formula_units_Z            2
_cell_length_a                   15.486
_cell_length_b                   16.747
_cell_length_c                   17.967
_cell_measurement_reflns_used    9841
_cell_measurement_temperature    90
_cell_measurement_theta_max      22.518
_cell_measurement_theta_min      2.586
_cell_volume                     4655.132
_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 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.1422
_diffrn_reflns_av_unetI/netI     0.1027
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            89558
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        23.138
_diffrn_reflns_theta_max         23.138
_diffrn_reflns_theta_min         1.134
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.460
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_correction_T_min  0.5908
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1251 before and 0.0904 after correction.
The Ratio of minimum to maximum transmission is 0.7931.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_description       prism
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.896
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1013
_refine_ls_number_reflns         12995
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1704
_refine_ls_R_factor_gt           0.0932
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0565P)^2^+56.0423P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2132
_refine_ls_wR_factor_ref         0.2594
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7390
_reflns_number_total             12995
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00911f2.cif
_cod_data_source_block           ls466-copy-copy
_cod_original_cell_volume        4655.1
_cod_database_code               7701660
_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:
 C01F(H01Y,H), C01S(H2CA,HE), C01T(H01O,H01P), C01Y(H01V,H01X), C01Z(H01Q,
 H01R), C020(H3CA,HH), C021(H02P,H02Q), C02G(H0BA,HV)
2.b Aromatic/amide H refined with riding coordinates:
 C017(H017), C01B(H7BA), C01C(H01C), C01E(H8BA), C01G(H01G), C01H(H9BA),
 C01K(H01Z), C01V(H5AA), C01W(H01W), C01X(H6AA), C025(H025), C02C(H02)
2.c Idealised Me refined as rotating group:
 C01I(H01A,H01B,H01D), C01L(H01E,H01F,H01H), C01M(H0CA,HA,HB), C01N(H01I,H01J,
 H01K), C01P(H01L,H01M,H01N), C01Q(H01S,H01T,H01U), C01R(H1CA,HC,HD), C01U(H01,
 HF,HG), C022(H02A,H02B,H02C), C023(H7AA,HI,HJ), C024(H02R,H02S,H02T),
 C026(H02U,H02V,H02W), C027(H02X,H02Y,HK), C028(H02Z,HL,HM), C029(H8AA,HN,HO),
 C02A(H9AA,HP,HQ), C02B(H02D,H02E,H02F), C02D(H0AA,HR,HS), C02E(H02G,H02H,H02I),
  C02F(H1AA,HT,HU), C02H(H2AA,HW,HX), C02I(H4CA,HY,HZ), C02J(H5CA,H2DA,H3DA),
 C02K(H1BA,H4DA,H5DA), C02L(H6CA,H6DA,H7DA), C02M(H7CA,H8DA,H9DA), C02N(H02J,
 H02K,H02L), C02O(H2BA,H0EA,H1EA), C02P(H3AA,H2EA,H3EA), C02Q(H3BA,H4EA,H5EA),
 C02R(H8CA,H6EA,H7EA), C02S(H4BA,H8EA,H9EA), C02T(H4AA,H0FA,H1FA), C02U(H9CA,
 H2FA,H3FA), C02V(H02M,H02N,H02O), C02W(H5BA,H4FA,H5FA), C02X(H0DA,H6FA,H7FA),
 C02Y(H1DA,H8FA,H9FA), C02Z(H6BA,H0GA,H1GA), C030(H03A,H03B,H03C)
;
_shelx_res_checksum              18507
_shelx_shelxl_version_number     2014/7
_olex2_submission_original_sample_id mp-136
_olex2_submission_special_instructions 'No special instructions were received'