1,3,4-Azadiphospholides as building blocks for scorpionate and bidentate ligands in multinuclear complexes.
Suter, Riccardo; Wagner, Mona; Querci, Lorenzo; Conti, Riccardo; Benkő, Zoltán; Grützmacher, Hansjörg; Dalton transactions (Cambridge, England : 2003) 49 (2020) 8201–8208; doi:10.1039/d0dt01864c

data_7704514
_publ_section_title
;
 1,3,4-Azadiphospholides as building blocks for scorpionate and bidentate
 ligands in multinuclear complexes.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8201
_journal_page_last               8208
_journal_paper_doi               10.1039/d0dt01864c
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C23 H17 N3 O3 P6 Ti, C7 H8'
_chemical_formula_sum            'C30 H25 N3 O3 P6 Ti'
_chemical_formula_weight         709.25
_chemical_name_systematic
Titanium(tris(1,3,4-azadiphospholo-1,2-pyridin-3-olate))-cyclopentadiene
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2016-06-09
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-07-19 deposited with the CCDC.	2020-05-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.1587(2)
_cell_length_b                   20.1174(3)
_cell_length_c                   24.1036(4)
_cell_measurement_reflns_used    11287
_cell_measurement_temperature    104.7(10)
_cell_measurement_theta_max      29.7250
_cell_measurement_theta_min      3.1310
_cell_volume                     6380.68(17)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      104.7(10)
_diffrn_detector                 'Oxford Diffraction Sapphire 3'
_diffrn_detector_area_resol_mean 8.26
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega   -6.00   20.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.7904  -99.0000   60.0000 26

  2 omega  -52.00   41.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.7904   77.0000 -150.0000 93

  3 omega  -89.00  -63.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.7904  161.0000 -148.0000 26

  4 omega   13.00   87.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2592   57.0000  -60.0000 74
;
_diffrn_measurement_device       'kappa-stage diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur S'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_UB_11      0.0155916000
_diffrn_orient_matrix_UB_12      0.0046234000
_diffrn_orient_matrix_UB_13      -0.0278943000
_diffrn_orient_matrix_UB_21      -0.0515763000
_diffrn_orient_matrix_UB_22      0.0016997000
_diffrn_orient_matrix_UB_23      -0.0084314000
_diffrn_orient_matrix_UB_31      0.0004449000
_diffrn_orient_matrix_UB_32      0.0349275000
_diffrn_orient_matrix_UB_33      0.0040854000
_diffrn_radiation_monochromator  'focusing graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_unetI/netI     0.0599
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            30300
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.283
_diffrn_reflns_theta_min         3.059
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.606
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.99290
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark violet'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_description       block
_exptl_crystal_F_000             2896
_exptl_crystal_preparation
'Cyclopentadienyltitaniumtrichloride and sodium azadiphospholate in toluene'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene'
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.501
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details
;
 Flack x determined using 4898 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.010(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     777
_refine_ls_number_reflns         15821
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0521
_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^)+(0.0464P)^2^+2.8533P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1083
_refine_ls_wR_factor_ref         0.1141
_reflns_Friedel_coverage         0.832
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                13534
_reflns_number_total             15821
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01864c2.cif
_cod_data_source_block           rs2_197
_cod_depositor_comments
'Adding full bibliography for 7704506--7704517.cif.'
_cod_database_code               7704514
_chemical_oxdiff_formula         'Ti1 P4 O2 N2 C50 H50 Cl2'
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C36(H36), C21(H21), C29(H29), C30(H30), C24(H24), C43(H43), C33(H33),
 C27(H27), C35(H35), C44(H44), C28(H28), C45(H45), C34(H34), C23(H23), C22(H22),
  C42(H42), C46(H46), C12(H12), C9(H9), C3(H3), C5(H5), C37(H37), C10(H10),
 C4(H4), C16(H16), C6(H6), C38(H38), C41(H41), C18(H18), C17(H17), C56(H56),
 C15(H15), C57(H57), C11(H11), C39(H39), C59(H59), C40(H40), C58(H58), C60(H60),
  C52(H52), C50(H50), C49(H49), C51(H51), C53(H53)
2.b Idealised Me refined as rotating group:
 C54(H54A,H54B,H54C), C47(H47A,H47B,H47C)
;
_shelx_res_checksum              72226
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2013-10-01
_olex2_submission_special_instructions 'No special instructions were received'