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_7704507
_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         'C26 H17 Mo N3 O6 P6 Ti, C4 H8 O1'
_chemical_formula_sum            'C30 H25 Mo N3 O7 P6 Ti'
_chemical_formula_weight         869.19
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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                 93.440(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.0367(3)
_cell_length_b                   19.6039(7)
_cell_length_c                   15.6787(6)
_cell_measurement_reflns_used    6202
_cell_measurement_temperature    100
_cell_measurement_theta_max      32.3140
_cell_measurement_theta_min      3.1050
_cell_volume                     3386.2(2)
_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      100
_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 0.999
_diffrn_measurement_details
;
  1 omega -102.00  -61.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.2303 -179.0000  120.0000 41

  2 omega  -97.00  -61.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.2303 -179.0000   30.0000 36

  3 omega -101.00  -61.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.2303 -179.0000 -150.0000 40

  4 omega  -35.00   97.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6990    0.0000    0.0000 132

  5 omega  -96.00  -27.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.2303  -77.0000  120.0000 69
;
_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      0.0168847000
_diffrn_orient_matrix_UB_12      0.0189386000
_diffrn_orient_matrix_UB_13      -0.0359462000
_diffrn_orient_matrix_UB_21      -0.0409474000
_diffrn_orient_matrix_UB_22      0.0262765000
_diffrn_orient_matrix_UB_23      0.0101571000
_diffrn_orient_matrix_UB_31      0.0467754000
_diffrn_orient_matrix_UB_32      0.0161299000
_diffrn_orient_matrix_UB_33      0.0256171000
_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  0.0676
_diffrn_reflns_av_unetI/netI     0.1100
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25661
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         2.781
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.941
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98790
_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 green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.705
_exptl_crystal_description       block
_exptl_crystal_F_000             1744
_exptl_crystal_preparation       'From saturated THF solution at RT'
_exptl_crystal_recrystallization_method 'From saturated THF solution at RT'
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.469
_refine_diff_density_min         -0.763
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     449
_refine_ls_number_reflns         10325
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.1032
_refine_ls_R_factor_gt           0.0563
_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^)+(0.0246P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0825
_refine_ls_wR_factor_ref         0.0926
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6988
_reflns_number_total             10325
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01864c2.cif
_cod_data_source_block           rs3104
_cod_depositor_comments
'Adding full bibliography for 7704506--7704517.cif.'
_cod_original_cell_volume        3386.17(19)
_cod_database_code               7704507
_chemical_oxdiff_formula         'Mo1 Ti1 P6 O6 N6 C50 H50'
_reflns_odcompleteness_completeness 99.87
_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
2. Restrained distances
 C27-O7 \\sim O8-C34 \\sim O8-C31 \\sim C27-C28
 with sigma of 0.02
 C30-O7 \\sim C30-C29 \\sim C29-C28 \\sim C32-C31 \\sim C32-C33 \\sim C33-C34
 with sigma of 0.002
 O8-C34 \\sim O7-C30 \\sim O8-C31 \\sim O7-C27
 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
Uanis(C27) = Uanis(C31)
Uanis(C28) = Uanis(C32)
Uanis(C29) = Uanis(C33)
Uanis(C30) = Uanis(C34)
Uanis(O7) = Uanis(O8)
4. Rigid body (RIGU) restrains
 C28, C27, C29, O7, C30
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C32, C33, C34, O8, C31
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(C33)=Sof(H33A)=
 Sof(H33B)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(O8)=1-FVAR(1)
 Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(C29)=Sof(H29A)=
 Sof(H29B)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(O7)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C27(H27A,H27B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,
 H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C16(H16), C9(H9), C11(H11), C6(H6), C18(H18), C20(H20), C12(H12),
 C21(H21), C15(H15), C22(H22), C19(H19), C4(H4), C5(H5), C10(H10), C17(H17),
 C1A(H1A)
;
_shelx_res_checksum              23444
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2014-03-05
_olex2_submission_special_instructions 'No special instructions were received'