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_7704510
_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
'C36 H24 N6 O6 P12 Ti, 2(C12 H30 Na O6), 2(C H2 Cl2)'
_chemical_formula_sum            'C62 H88 Cl4 N6 Na2 O18 P12 Ti'
_chemical_formula_weight         1812.70
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2016-07-19
_audit_creation_method
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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
;
2016-07-19 deposited with the CCDC.	2020-05-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.1170(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.9086(7)
_cell_length_b                   24.9553(13)
_cell_length_c                   13.7959(7)
_cell_measurement_reflns_used    8622
_cell_measurement_temperature    99(2)
_cell_measurement_theta_max      25.36
_cell_measurement_theta_min      2.50
_cell_volume                     4223.9(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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      99.55
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 8.33
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'fixed chi three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART Apex2'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0748
_diffrn_reflns_av_unetI/netI     0.0781
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            50291
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.086
_diffrn_reflns_theta_min         1.632
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.530
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_description       block
_exptl_crystal_F_000             1876
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.537
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.906
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         8349
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.906
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0374
_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^)+(0.0278P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0642
_refine_ls_wR_factor_ref         0.0710
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5616
_reflns_number_total             8349
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01864c2.cif
_cod_data_source_block           a
_cod_depositor_comments
'Adding full bibliography for 7704506--7704517.cif.'
_cod_database_code               7704510
_shelx_estimated_absorpt_t_max   0.934
_shelx_estimated_absorpt_t_min   0.911
_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:
 C24(H24A,H24B), C25(H25A,H25B), C28(H28A,H28B), C29(H29A,H29B), C21(H21A,
 H21B), C20(H20A,H20B), C31(H31A,H31B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C17(H17), C11(H11), C9(H9), C4(H4), C15(H15), C18(H18), C3(H3),
 C16(H16), C12(H12), C5(H5), C10(H10)
2.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C30(H30A,H30B,H30C), C26(H26A,H26B,H26C), C23(H23A,H23B,
 H23C), C19(H19A,H19B,H19C), C22(H22A,H22B,H22C)
;
_shelx_res_checksum              97582
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'