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_7704508
_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
'0.25(C84 H127.75 Mo4 N12 O16 P12), 0.87(C H2 Cl2), 0.5(C0.98 H2 Cl2)'
_chemical_formula_sum            'C22.36 H35.49 Cl2.75 Mo N3 O4 P3'
_chemical_formula_weight         696.76
_chemical_melting_point          471
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-07-20
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
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
_cell_formula_units_Z            32
_cell_length_a                   59.1004(11)
_cell_length_b                   34.6994(6)
_cell_length_c                   12.38327(19)
_cell_measurement_reflns_used    13414
_cell_measurement_temperature    106.05(13)
_cell_measurement_theta_max      31.7750
_cell_measurement_theta_min      3.3410
_cell_volume                     25395.0(8)
_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_environment      N~2~
_diffrn_ambient_temperature      106.05(13)
_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  -80.00  -33.00   0.5000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3865  127.0000  -43.0000 94

  2 omega  -31.00   41.00   0.5000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3865   57.0000  -60.0000 144

  3 omega  -43.00   51.00   0.5000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8553  -19.0000  -30.0000 188

  4 omega -103.00  -70.00   0.5000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3865 -179.0000   90.0000 66
;
_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      0.0019117000
_diffrn_orient_matrix_UB_12      0.0200754000
_diffrn_orient_matrix_UB_13      0.0054380000
_diffrn_orient_matrix_UB_21      -0.0118295000
_diffrn_orient_matrix_UB_22      0.0033614000
_diffrn_orient_matrix_UB_23      -0.0025006000
_diffrn_orient_matrix_UB_31      -0.0007084000
_diffrn_orient_matrix_UB_32      -0.0017793000
_diffrn_orient_matrix_UB_33      0.0569757000
_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  0.0374
_diffrn_reflns_av_unetI/netI     0.0436
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       78
_diffrn_reflns_limit_h_min       -67
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            32415
_diffrn_reflns_point_group_measured_fraction_full 0.789
_diffrn_reflns_point_group_measured_fraction_max 0.762
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         2.963
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.827
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97741
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_description       block
_exptl_crystal_F_000             11406
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: DCM'
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.196
_refine_diff_density_min         -0.622
_refine_diff_density_rms         0.102
_refine_ls_abs_structure_details
;
 Flack x determined using 3237 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.05(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     672
_refine_ls_number_reflns         12027
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0471
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0494P)^2^+185.0356P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1077
_refine_ls_wR_factor_ref         0.1093
_reflns_Friedel_coverage         0.460
_reflns_Friedel_fraction_full    0.558
_reflns_Friedel_fraction_max     0.503
_reflns_number_gt                11466
_reflns_number_total             12027
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01864c2.cif
_cod_data_source_block           rs4082b
_cod_depositor_comments
'Adding full bibliography for 7704506--7704517.cif.'
_cod_original_cell_volume        25394.9(8)
_cod_database_code               7704508
_chemical_oxdiff_formula         P3N3Mo1O6C50H50
_reflns_odcompleteness_completeness 99.77
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(Cl6S) = Uanis(Cl5S)
Uanis(Cl7S) = Uanis(Cl8S)
Uanis(Cl1) = Uanis(C0AA) = Uanis(Cl3)
3. Others
 Sof(H3SC)=Sof(H3SD)=Sof(Cl6S)=Sof(Cl7S)=1-FVAR(1)
 Sof(Cl8S)=Sof(Cl5S)=Sof(H3SA)=Sof(H3SB)=FVAR(1)
 Sof(Cl4S)=Sof(Cl3S)=Sof(C2S)=Sof(H2SA)=Sof(H2SB)=FVAR(2)
 Sof(H17A)=Sof(H17B)=Sof(H17C)=FVAR(3)
4.a Ternary CH refined with riding coordinates:
 C10(H10), C13A(H13A), C10A(H10A), C7A(H7A), C7(H7), C16A(H16A), C13(H13),
 C16(H16)
4.b Secondary CH2 refined with riding coordinates:
 C3S(H3SA,H3SB), C3S(H3SC,H3SD), C2S(H2SA,H2SB), C0AA(H0AA,H0AB)
4.c Aromatic/amide H refined with riding coordinates:
 C5A(H5A), C5(H5), C4A(H4A), C6(H6), C6A(H6A), C4(H4), C3A(H3A), C3(H3)
4.d Idealised Me refined as rotating group:
 C17A(H17A,H17B,H17C), C9(H9A,H9B,H9C), C11A(H11A,H11B,H11C), C11(H11D,H11E,
 H11F), C8A(H8AA,H8AB,H8AC), C15A(H15A,H15B,H15C), C12(H12A,H12B,H12C),
 C12A(H12D,H12E,H12F), C18A(H18A,H18B,H18C), C14A(H14A,H14B,H14C), C8(H8A,H8B,
 H8C), C9A(H9AA,H9AB,H9AC), C17(H17D,H17E,H17F), C18(H18D,H18E,H18F), C15(H15D,
 H15E,H15F), C14(H14D,H14E,H14F)
;
_shelx_res_checksum              33319
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'