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_7704515
_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, C H2 Cl2'
_chemical_formula_sum            'C24 H19 Cl2 N3 O3 P6 Ti'
_chemical_formula_weight         702.04
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_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             2016-07-19
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Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
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_audit_update_record
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2016-07-19 deposited with the CCDC.	2020-05-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.364(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_length_c                   26.3095(15)
_cell_measurement_reflns_used    6302
_cell_measurement_temperature    104.6(2)
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_cell_volume                     2979.7(3)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
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_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      104.6(2)
_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 0.926
_diffrn_measurement_details
;
  1 omega  -46.00   31.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -31.6391   38.0000 -120.0000 77

  2 omega  -93.00  -34.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -31.6391 -179.0000 -150.0000 59

  3 omega   66.00  108.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1078 -158.0000   85.0000 42

  4 omega   81.00  107.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1078  179.0000 -180.0000 26

  5 omega   27.00  101.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1078   57.0000   90.0000 74

  6 omega   12.00   47.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1078   57.0000  -90.0000 35
;
_diffrn_measurement_device       'kappa-stage diffractometer'
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_diffrn_orient_matrix_UB_22      0.0098270000
_diffrn_orient_matrix_UB_23      0.0261292000
_diffrn_orient_matrix_UB_31      0.0952091000
_diffrn_orient_matrix_UB_32      -0.0007111000
_diffrn_orient_matrix_UB_33      0.0036640000
_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  0.0526
_diffrn_reflns_av_unetI/netI     0.0806
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.926
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_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            26042
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.926
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         34.885
_diffrn_reflns_theta_min         3.053
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.822
_exptl_absorpt_correction_T_max  1.00000
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_exptl_absorpt_correction_type   multi-scan
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;
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 green'
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_description       block
_exptl_crystal_F_000             1416
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.327
_refine_diff_density_min         -1.583
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         12040
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0990
_refine_ls_R_factor_gt           0.0671
_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^)+(0.0911P)^2^+0.9700P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1633
_refine_ls_wR_factor_ref         0.1938
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8888
_reflns_number_total             12040
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01864c2.cif
_cod_data_source_block           rs3023_green
_cod_depositor_comments
'Adding full bibliography for 7704506--7704517.cif.'
_cod_database_code               7704515
_chemical_oxdiff_formula         'P8 O4 N4 Ti Na O10 C40 H40'
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     33.07
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B)
2.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C18(H18), C11(H11), C6(H6), C15(H15), C17(H17), C16(H16), C9(H9),
 C10(H10), C5(H5), C23(H23), C22(H22), C3(H3), C4(H4), C21(H21), C20(H20),
 C19(H19)
;
_shelx_res_checksum              82287
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'