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_7704512
_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         'C18 H32 N3 O P3'
_chemical_formula_sum            'C18 H32 N3 O P3'
_chemical_formula_weight         399.37
_chemical_melting_point          421
_chemical_name_systematic
1-([1,3,4]azadiphospholo[1,2-a]pyridin-3-yloxy)-N,N,N',N'-tetraisopropylphosphanediamine
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
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Olex2 1.2
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2016-07-21 deposited with the CCDC.	2020-05-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
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_cell_length_b                   11.3677(4)
_cell_length_c                   29.4791(17)
_cell_measurement_reflns_used    4703
_cell_measurement_temperature    104.79(12)
_cell_measurement_theta_max      30.3350
_cell_measurement_theta_min      3.1920
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_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
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_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      104.79(12)
_diffrn_detector                 'Oxford Diffraction Sapphire 3'
_diffrn_detector_area_resol_mean 8.26
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.889
_diffrn_measurement_details
;
  1 omega  -12.00   14.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.7904  -99.0000   90.0000 26

  2 omega  -50.00   80.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2592    0.0000 -150.0000 130
;
_diffrn_measurement_device       'kappa-stage diffractometer'
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_diffrn_orient_matrix_UB_23      -0.0045252000
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_diffrn_orient_matrix_UB_32      -0.0518369000
_diffrn_orient_matrix_UB_33      0.0087030000
_diffrn_radiation_monochromator  'focusing graphite'
_diffrn_radiation_probe          x-ray
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_diffrn_reflns_av_R_equivalents  0.0210
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_Laue_measured_fraction_full 0.999
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_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            14270
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.889
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.575
_diffrn_reflns_theta_min         3.151
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.286
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98176
_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            'clear light yellow'
_exptl_crystal_density_diffrn    1.224
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_exptl_crystal_F_000             1712
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene'
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_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     234
_refine_ls_number_reflns         5923
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0310P)^2^+2.0790P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0844
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_reflns_number_gt                5195
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_reflns_threshold_expression     'I > 2\s(I)'
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_cod_data_source_block           rs2097
_cod_depositor_comments
'Adding full bibliography for 7704506--7704517.cif.'
_cod_database_code               7704512
_chemical_oxdiff_formula         'P3 N3 C40 H40'
_reflns_odcompleteness_completeness 99.68
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_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 Ternary CH refined with riding coordinates:
 C14(H14), C7(H7), C8(H8), C13(H13)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C5(H5), C4(H4), C3(H3)
2.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C17(H17A,H17B,H17C), C16(H16A,H16B,H16C), C11(H11A,H11B,
 H11C), C10(H10A,H10B,H10C), C15(H15A,H15B,H15C), C9(H9A,H9B,H9C), C12(H12A,
 H12B,H12C)
;
_shelx_res_checksum              17727
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'