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_7704517
_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 Hf N6 O6 P12, 2(C12 H30 Na O6)'
_chemical_formula_sum            'C60 H84 Hf N6 Na2 O18 P12'
_chemical_formula_weight         1773.44
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-10-14
_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                90.00
_cell_angle_beta                 90.052(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.9451(3)
_cell_length_b                   13.2815(2)
_cell_length_c                   18.8611(5)
_cell_measurement_reflns_used    4727
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.5090
_cell_measurement_theta_min      2.9780
_cell_volume                     3994.30(14)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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      293(2)
_diffrn_detector_area_resol_mean 16.0839
_diffrn_measured_fraction_theta_full 0.900
_diffrn_measured_fraction_theta_max 0.898
_diffrn_measurement_details
;
  1 omega    2.00   97.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6990   38.0000  -60.0000 95

  2 omega   36.00   68.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6990   57.0000   60.0000 32

  3 omega   13.00   69.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6990  -99.0000  150.0000 56
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0381881000
_diffrn_orient_matrix_UB_12      0.0039967000
_diffrn_orient_matrix_UB_13      -0.0190894000
_diffrn_orient_matrix_UB_21      -0.0223068000
_diffrn_orient_matrix_UB_22      0.0043596000
_diffrn_orient_matrix_UB_23      0.0323938000
_diffrn_orient_matrix_UB_31      0.0046756000
_diffrn_orient_matrix_UB_32      0.0530723000
_diffrn_orient_matrix_UB_33      -0.0011985000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_unetI/netI     0.0629
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            13164
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.94
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.622
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.99154
_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_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1808
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DME/THF'
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.613
_refine_diff_density_min         -0.507
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         7328
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0415
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0270P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0723
_refine_ls_wR_factor_ref         0.0778
_reflns_number_gt                6042
_reflns_number_total             7328
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d0dt01864c2.cif
_cod_data_source_block           rs3033
_cod_depositor_comments
'Adding full bibliography for 7704506--7704517.cif.'
_cod_original_cell_volume        3994.33(14)
_cod_database_code               7704517
_chemical_oxdiff_formula         'Hf1 P4 O2 N2 C100 H100'
_reflns_odcompleteness_completeness 86.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_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), C20(H20A,H20B), C21(H21A,H21B), C28(H28A,
 H28B), C29(H29A,H29B)
2.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C10(H10), C11(H11), C6(H6), C12(H12), C3(H3), C4(H4), C15(H15),
 C9(H9), C16(H16), C5(H5), C17(H17)
2.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C22(H22A,H22B,H22C), C27(H27A,H27B,H27C), C19(H19A,H19B,
 H19C), C30(H30A,H30B,H30C), C26(H26A,H26B,H26C)
;
_olex2_submission_special_instructions 'No special instructions were received'