Anionic 1-Aza-3,4-diphospholides as redox active ligands
Suter, Riccardo; Gilliard, Robert J.; Iskandarov, Javad; Benkő, Zoltan; Wörle, Michael; Grützmacher, Hansjörg; Inorganica Chimica Acta 520 (2021) 120274–; doi:10.1016/j.ica.2021.120274

data_1566185
_publ_section_title
;
 Anionic 1-Aza-3,4-diphospholides as redox active ligands
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              120274
_journal_paper_doi               10.1016/j.ica.2021.120274
_journal_volume                  520
_journal_year                    2021
_chemical_formula_moiety         'C42 H52 Fe2 N2 O8 P4, C4 H10 O'
_chemical_formula_sum            'C46 H62 Fe2 N2 O9 P4'
_chemical_formula_weight         1022.55
_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
_atom_sites_solution_primary     direct
_cell_angle_alpha                103.7106(19)
_cell_angle_beta                 91.106(2)
_cell_angle_gamma                112.185(2)
_cell_formula_units_Z            2
_cell_length_a                   10.9061(3)
_cell_length_b                   14.4034(3)
_cell_length_c                   18.4848(5)
_cell_measurement_reflns_used    9720
_cell_measurement_temperature    106.8(4)
_cell_measurement_theta_max      32.0990
_cell_measurement_theta_min      1.6010
_cell_volume                     2592.93(12)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    OLEX2
_computing_publication_material  OLEX2
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      106.8(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0839
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -82.00 -36.00   1.00   10.00    --  -26.39 125.00 -28.00   46
  2  \w    -11.00  69.00   1.00   10.00    --   26.86 -99.00  60.00   80
  3  \w     36.00  84.00   1.00   10.00    --   26.86-125.00-106.00   48
  4  \w      6.00  96.00   1.00   10.00    --   26.86  57.00 -30.00   90
  5  \w    -40.00  48.00   1.00   10.00    --   26.86 -57.00  90.00   88
  6  \w    -14.00 100.00   1.00   10.00    --   26.86  19.00 -90.00  114
  7  \w     34.00 103.00   1.00   10.00    --   26.86 179.00 -60.00   69
  8  \w    -42.00 -17.00   1.00   10.00    --   26.86 -57.00 -60.00   25
  9  \w      6.00  96.00   1.00   10.00    --   26.86  57.00  90.00   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0051344000
_diffrn_orient_matrix_UB_12      0.0210728000
_diffrn_orient_matrix_UB_13      0.0392619000
_diffrn_orient_matrix_UB_21      -0.0333822000
_diffrn_orient_matrix_UB_22      -0.0507687000
_diffrn_orient_matrix_UB_23      0.0044970000
_diffrn_orient_matrix_UB_31      0.0621818000
_diffrn_orient_matrix_UB_32      -0.0043066000
_diffrn_orient_matrix_UB_33      0.0046508000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0455
_diffrn_reflns_av_unetI/netI     0.0611
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            40658
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.506
_diffrn_reflns_theta_min         1.583
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.734
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82418
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_description       block
_exptl_crystal_F_000             1072
_exptl_crystal_recrystallization_method 'crystallized from diethyl ether'
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.846
_refine_diff_density_min         -0.740
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     593
_refine_ls_number_reflns         15834
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0738
_refine_ls_R_factor_gt           0.0483
_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^)+(0.0538P)^2^+0.6853P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1083
_refine_ls_wR_factor_ref         0.1199
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                11668
_reflns_number_total             15834
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            5-syn.cif
_cod_data_source_block           rs5130
_cod_original_cell_volume        2592.92(12)
_cod_database_code               1566185
_chemical_oxdiff_formula         Fe2C47H59N2O9P4
_shelx_estimated_absorpt_t_max   0.855
_shelx_estimated_absorpt_t_min   0.719
_reflns_odcompleteness_completeness 99.99
_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. Rigid bond restraints
 O9, C1A, C1B, C1C, C1D
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
Uiso(C1E) = Uiso(C1F) = Uiso(O10) = Uiso(C1G) = Uiso(C1H)
Uiso(C1L) = Uiso(C1K) = Uiso(O11) = Uiso(C1J) = Uiso(C1I)
4. Rigid body (RIGU) restrains
 O9, C1A, C1B, C1C, C1D
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: C1A(0.5) H1AA(0.5) H1AB(0.5) H1AC(0.5) O9(0.5) C1B(0.5) H1BA(0.5)
 H1BB(0.5) C1C(0.5) H1CA(0.5) H1CB(0.5) C1D(0.5) H1DA(0.5) H1DB(0.5) H1DC(0.5)
 C1E(0.25) H1EA(0.25) H1EB(0.25) H1EC(0.25) O10(0.25) C1F(0.25) H1FA(0.25)
 H1FB(0.25) C1G(0.25) H1GA(0.25) H1GB(0.25) C1H(0.25) H1HA(0.25) H1HB(0.25)
 H1HC(0.25) C1I(0.25) H1IA(0.25) H1IB(0.25) H1IC(0.25) O11(0.25) C1J(0.25)
 H1JA(0.25) H1JB(0.25) C1K(0.25) H1KA(0.25) H1KB(0.25) C1L(0.25) H1LA(0.25)
 H1LB(0.25) H1LC(0.25)
6.a Free rotating group:
 C1A(O9,C1B,C1C,C1D), C1E(O10,C1F,C1G,C1H), C1I(O11,C1J,C1K,C1L)
6.b Ternary CH refined with riding coordinates:
 C9(H9), C16(H16), C27(H27), C34(H34)
6.c Secondary CH2 refined with riding coordinates:
 C1B(H1BA,H1BB), C1C(H1CA,H1CB), C1F(H1FA,H1FB), C1G(H1GA,H1GB), C1J(H1JA,
 H1JB), C1K(H1KA,H1KB)
6.d Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C30(H30), C31(H31), C32(H32)
6.e Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C10(H10A,H10B,H10C),
 C11(H11A,H11B,H11C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C28(H28A,H28B,H28C), C29(H29A,
 H29B,H29C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C1A(H1AA,H1AB,H1AC),
 C1D(H1DA,H1DB,H1DC), C1E(H1EA,H1EB,H1EC), C1H(H1HA,H1HB,H1HC), C1I(H1IA,H1IB,
 H1IC), C1L(H1LA,H1LB,H1LC)
;
_shelx_res_checksum              5216
_shelx_hkl_checksum              45646
_olex2_exptl_crystal_mounting_method tip-mounted
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.155
_oxdiff_exptl_absorpt_empirical_full_min 0.907