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_7704511
_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         'C24 H17 B N3 O3 P6, C12.46 H27.9 Na O4.4'
_chemical_formula_sum            'C36.46 H44.9 B N3 Na O7.4 P6'
_chemical_formula_weight         863.20
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-07-15
_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            4
_cell_length_a                   33.7644(14)
_cell_length_b                   12.0728(6)
_cell_length_c                   11.6209(5)
_cell_measurement_reflns_used    8830
_cell_measurement_temperature    106(9)
_cell_measurement_theta_max      22.7310
_cell_measurement_theta_min      3.3650
_cell_volume                     4737.0(4)
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      106(9)
_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  -88.00   26.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9802  -19.0000 -180.0000 114

  2 omega   52.00   82.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.4490  179.0000  120.0000 30

  3 omega   -3.00   38.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.4490   57.0000   30.0000 41

  4 omega  -50.00   40.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.4490  -57.0000 -120.0000 90

  5 omega  -94.00  -68.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9802  179.0000   60.0000 26

  6 omega  -87.00    3.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9802  -57.0000  120.0000 90
;
_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      -0.0091756000
_diffrn_orient_matrix_UB_12      0.0287251000
_diffrn_orient_matrix_UB_13      -0.0460957000
_diffrn_orient_matrix_UB_21      -0.0124859000
_diffrn_orient_matrix_UB_22      -0.0462516000
_diffrn_orient_matrix_UB_23      -0.0100537000
_diffrn_orient_matrix_UB_31      -0.0141776000
_diffrn_orient_matrix_UB_32      0.0221320000
_diffrn_orient_matrix_UB_33      0.0387099000
_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  0.1077
_diffrn_reflns_av_unetI/netI     0.0965
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            34644
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.945
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.281
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94389
_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 dark yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_description       block
_exptl_crystal_F_000             1799
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.727
_refine_diff_density_min         -0.652
_refine_diff_density_rms         0.105
_refine_ls_abs_structure_details
;
 Flack x determined using 1897 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.03(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         9513
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.1366
_refine_ls_R_factor_gt           0.1122
_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^)+(0.1630P)^2^+6.5040P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2802
_refine_ls_wR_factor_ref         0.3057
_reflns_Friedel_coverage         0.871
_reflns_Friedel_fraction_full    0.965
_reflns_Friedel_fraction_max     0.963
_reflns_number_gt                7128
_reflns_number_total             9513
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01864c2.cif
_cod_data_source_block           exp_4270
_cod_depositor_comments
'Adding full bibliography for 7704506--7704517.cif.'
_cod_original_cell_volume        4737.1(4)
_cod_original_formula_sum        'C36.46 H44.90 B N3 Na O7.40 P6'
_cod_database_code               7704511
_chemical_oxdiff_formula         Na1O9B1P6C50H50N3
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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, All C(H,H,H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O00X) = Uanis(Na07) = Uanis(O00L) = Uanis(O00W) = Uanis(O013) =
Uanis(O00K) = Uanis(C3) = Uanis(C01I) = Uanis(C01C) = Uanis(C01D) = Uanis(C01G)
= Uanis(C01A) = Uanis(C19) = Uanis(C019) = Uanis(C6) = Uanis(C14) = Uanis(C01H)
Uanis(O2) = Uanis(C6AA) = Uanis(C5) = Uanis(C8) = Uanis(C5AA) = Uanis(O3) =
Uanis(C11) = Uanis(C12) = Uanis(C15) = Uanis(C16)
Uanis(C7AA) = Uanis(C10) = Uanis(C4) = Uanis(O1)
3. Rigid body (RIGU) restrains
 O2, C6AA, C5, C8, C5AA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O3, C11, C12, C15, C16
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(O00L)=Sof(O00W)=Sof(O013)=Sof(C019)=Sof(H01A)=Sof(H01B)=Sof(C01A)=
 Sof(H01C)=Sof(H01D)=Sof(H01E)=Sof(C01H)=Sof(H01M)=Sof(H01N)=Sof(C01I)=
 Sof(H01O)=Sof(H01P)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C6)=Sof(H6A)=Sof(H6B)=
 Sof(H6C)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(C19)=Sof(H19A)=Sof(H19B)=FVAR(1)
 Sof(O00K)=Sof(O00X)=Sof(C01C)=Sof(H01F)=Sof(H01G)=Sof(H01H)=Sof(C01D)=
 Sof(H01I)=Sof(H01J)=Sof(C01G)=Sof(H01K)=Sof(H01L)=Sof(H3AD)=Sof(H3AE)=
 Sof(H3AF)=FVAR(2)
 Fixed Sof: H3AA(0.33333) H3AB(0.33333) H3AC(0.33333) O2(0.5) C6AA(0.5)
 H6AA(0.5) H6AB(0.5) C5(0.5) H5A(0.5) H5B(0.5) C8(0.5) H8A(0.5) H8B(0.5)
 C5AA(0.5) H5AA(0.5) H5AB(0.5) O3(0.5) C11(0.5) H11A(0.5) H11B(0.5) C12(0.5)
 H12A(0.5) H12B(0.5) C15(0.5) H15A(0.5) H15B(0.5) C16(0.5) H16A(0.5) H16B(0.5)
 O1(0.33333) C7AA(0.25) H7AA(0.25) H7AB(0.25) H7AC(0.25) C4(0.25) H4A(0.25)
 H4B(0.25) C10(0.25) H10A(0.25) H10B(0.25)
5.a Free rotating group:
 O2(C6AA,C5,C8,C5AA), O3(C11,C12,C15,C16,O1,C7AA)
5.b Secondary CH2 refined with riding coordinates:
 C019(H01A,H01B), C01D(H01I,H01J), C01G(H01K,H01L), C01H(H01M,H01N), C01I(H01O,
 H01P), C3(H3A,H3B), C14(H14A,H14B), C19(H19A,H19B), C6AA(H6AA,H6AB), C5(H5A,
 H5B), C8(H8A,H8B), C5AA(H5AA,H5AB), C11(H11A,H11B), C12(H12A,H12B), C15(H15A,
 H15B), C16(H16A,H16B), C4(H4A,H4B), C10(H10A,H10B)
5.c Me refined with riding coordinates:
 C3AA(H3AD,H3AE,H3AF)
5.d Aromatic/amide H refined with riding coordinates:
 C00H(H00H), C00I(H00I), C00N(H00N), C00O(H00O), C00P(H00P), C00Q(H00Q),
 C00U(H00U), C00Z(H00Z), C010(H010), C011(H011), C012(H012), C014(H014),
 C016(H016), C2AA(H2AA), C0(H0), C4AA(H4AA), C2(H2)
5.e Idealised Me refined with everything fixed:
 C7AA(H7AA,H7AB,H7AC)
5.f Idealised Me refined as rotating group:
 C01A(H01C,H01D,H01E), C01C(H01F,H01G,H01H), C6(H6A,H6B,H6C), C3AA(H3AA,H3AB,
 H3AC)
;
_shelx_res_checksum              36859
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'