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_7704516
_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
'C42 H24 Hf Mo2 N6 O12 P12, 2(C12 H30 Na O6), 2(C H1.93 Cl1.96)'
_chemical_formula_sum            'C68 H87.86 Cl3.92 Hf Mo2 N6 Na2 O24 P12'
_chemical_formula_weight         2300.25
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-07-19
_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                83.345(2)
_cell_angle_beta                 68.758(2)
_cell_angle_gamma                60.501(3)
_cell_formula_units_Z            1
_cell_length_a                   13.1135(3)
_cell_length_b                   13.1212(4)
_cell_length_c                   16.9409(4)
_cell_measurement_reflns_used    24574
_cell_measurement_temperature    104(2)
_cell_measurement_theta_max      30.8810
_cell_measurement_theta_min      3.2230
_cell_volume                     2357.65(13)
_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      104(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 0.891
_diffrn_measurement_details
;
  1 omega  -91.00  -64.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.8987 -179.0000   30.0000 27

  2 omega  -24.00   15.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.8987  -99.0000  150.0000 39

  3 omega  -25.00   20.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.8987  -99.0000  -90.0000 45

  4 omega  -20.00   16.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.8987  -99.0000   30.0000 36

  5 omega  -36.00   27.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.8987   38.0000  -90.0000 63

  6 omega  -81.00   49.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.8987    0.0000 -150.0000 130

  7 omega  -36.00   36.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.8987   57.0000   30.0000 72

  8 omega  -86.00   -2.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.8987  -57.0000 -180.0000 84

  9 omega  -38.00   50.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.8987   38.0000  -30.0000 88

 10 omega    3.00   48.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       19.3674   57.0000   30.0000 45
;
_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      -0.0511251000
_diffrn_orient_matrix_UB_12      -0.0063524000
_diffrn_orient_matrix_UB_13      0.0288080000
_diffrn_orient_matrix_UB_21      0.0189160000
_diffrn_orient_matrix_UB_22      -0.0499199000
_diffrn_orient_matrix_UB_23      -0.0253585000
_diffrn_orient_matrix_UB_31      0.0379551000
_diffrn_orient_matrix_UB_32      -0.0367187000
_diffrn_orient_matrix_UB_33      0.0236007000
_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  0.0236
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.891
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            38086
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.891
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.000
_diffrn_reflns_theta_min         3.031
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.754
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93975
_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 orange'
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_description       plate
_exptl_crystal_F_000             1154
_exptl_crystal_size_max          0.912
_exptl_crystal_size_mid          0.479
_exptl_crystal_size_min          0.393
_refine_diff_density_max         0.663
_refine_diff_density_min         -0.548
_refine_diff_density_rms         0.072
_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     564
_refine_ls_number_reflns         13365
_refine_ls_number_restraints     534
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0253
_refine_ls_R_factor_gt           0.0230
_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^)+(0.0233P)^2^+0.9960P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0529
_refine_ls_wR_factor_ref         0.0538
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12528
_reflns_number_total             13365
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01864c2.cif
_cod_data_source_block           rs3155
_cod_depositor_comments
'Adding full bibliography for 7704506--7704517.cif.'
_cod_original_cell_volume        2357.64(12)
_cod_database_code               7704516
_chemical_oxdiff_formula         'Mo1 Hf1 P6 N3 C50 H50 O12'
_chemical_oxdiff_usercomment     '0.12 0.22 0.16'
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(HC)=Sof(HD)=Sof(Cl2A)=1-FVAR(1)
 Sof(Cl2)=FVAR(1)
 Sof(Cl00)=Sof(H1AA)=Sof(HB)=Sof(Cl)=FVAR(2)
4.a Secondary CH2 refined with riding coordinates:
 C01D(H01N,H01O), C01E(H01P,H01Q), C01I(H01U,H01V), C01J(H01W,H01X), C01L(H1AA,
 HB), C01L(HC,HD), C01M(H01Z,HE), C01N(H01,HF)
4.b Aromatic/amide H refined with riding coordinates:
 C00T(H00T), C00Y(H00Y), C00Z(H00Z), C014(H014), C015(H015), C016(H016),
 C017(H017), C018(H018), C01B(H01B), C01C(H01C), C01F(H01F), C01G(H01G)
4.c Idealised Me refined as rotating group:
 C011(H01A,H01D,H01E), C013(H01H,H01I,H01J), C01A(H01K,H01L,H01M), C01H(H01R,
 H01S,H01T), C01K(H01Y,H,HA), C01O(H0AA,HG,HH)
;
_shelx_res_checksum              74616
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'