Crystalline phosphino-functionalized mesoionic olefins (p-MIOs)
Merschel, Arne; Vishnevskiy, Yury V.; Neumann, Beate; Stammler, Georg; Ghadwal, Rajendra S.; Dalton Transactions  (2022) –; doi:10.1039/D2DT01314B

data_7710158
_publ_section_title
;
 Crystalline phosphino-functionalized mesoionic olefins (p-MIOs)
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01314B
_journal_year                    2022
_chemical_formula_moiety         'C92 H102 Au2 N4 P2, 2(Cl), 5[CH2Cl2]'
_chemical_formula_sum            'C97 H112 Au2 Cl12 N4 P2'
_chemical_formula_weight         2215.17
_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     dual
_audit_creation_date             2020-06-03
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2021-11-12 deposited with the CCDC.	2022-05-02 downloaded from the CCDC.
;
_cell_angle_alpha                95.2343(15)
_cell_angle_beta                 105.4602(15)
_cell_angle_gamma                90.6853(15)
_cell_formula_units_Z            1
_cell_length_a                   12.5519(2)
_cell_length_b                   13.5059(3)
_cell_length_c                   17.4784(3)
_cell_measurement_reflns_used    45752
_cell_measurement_temperature    99.97(13)
_cell_measurement_theta_max      32.6050
_cell_measurement_theta_min      3.0020
_cell_volume                     2841.87(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.77a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.77a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.77a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.97(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.924
_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    -42.00  13.00   1.00   30.00    --  -17.14 -77.00 150.00   55
  2  \w    -91.00 -43.00   1.00   30.00    --  -17.14 154.00 -21.08   48
  3  \w    -54.00  38.00   1.00   30.00    --   17.14 -38.00 -30.00   92
  4  \w     -4.00  88.00   1.00   30.00    --   17.14  38.00 150.00   92
  5  \w    -51.00  42.00   1.00   30.00    --   17.14 -57.00  30.00   93
  6  \w    -29.00  53.00   1.00   30.00    --   17.14 -90.00-132.62   82
  7  \w     -8.00  86.00   1.00   30.00    --   17.14  57.00  30.00   94
  8  \w    -51.00  42.00   1.00   30.00    --   17.14 -57.00 120.00   93
  9  \w     -8.00  86.00   1.00   30.00    --   17.14  57.00 -60.00   94
 10  \w      7.00  72.00   1.00   30.00    --   17.14-126.00   2.74   65
 11  \w    -76.00 -30.00   1.00   30.00    --  -17.14 132.00  76.66   46
 12  \w    -42.00  13.00   1.00   30.00    --  -17.14 -77.00   0.00   55
 13  \w      9.00  68.00   1.00   30.00    --   17.14-132.00 -71.92   59
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0166912000
_diffrn_orient_matrix_UB_12      0.0404958000
_diffrn_orient_matrix_UB_13      0.0223619000
_diffrn_orient_matrix_UB_21      -0.0525607000
_diffrn_orient_matrix_UB_22      -0.0022054000
_diffrn_orient_matrix_UB_23      -0.0282534000
_diffrn_orient_matrix_UB_31      -0.0200420000
_diffrn_orient_matrix_UB_32      -0.0337753000
_diffrn_orient_matrix_UB_33      0.0221793000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0551
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.924
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            89437
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.890
_diffrn_reflns_theta_min         2.558
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.928
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.308
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.77a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1114
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.171
_exptl_crystal_size_min          0.135
_refine_diff_density_max         4.486
_refine_diff_density_min         -2.402
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         19635
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0458
_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^)+(0.0599P)^2^+6.5325P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1183
_refine_ls_wR_factor_ref         0.1228
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17539
_reflns_number_total             19635
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01314b2.cif
_cod_data_source_block           compound_5xCl
_cod_database_code               7710158
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C102 H112 Au2 Cl12 N4 P2'
_shelx_estimated_absorpt_t_max   0.693
_shelx_estimated_absorpt_t_min   0.410
_diffrn_oxdiff_digest_frames
;
01c6ce6cbe192590d287fffd25c051f9b60097249f9
;
_diffrn_oxdiff_digest_hkl
;
018047237daf0c6227c879d8302ed72e681eac
;
_reflns_odcompleteness_completeness 99.86
_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
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C10(H10), C13(H13), C22(H22), C25(H25)
2.b Secondary CH2 refined with riding coordinates:
 C34(H34A,H34B)
2.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C18(H18), C19(H19), C20(H20), C29(H29), C30(H30),
 C31(H31), C32(H32), C33(H33), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40),
  C42(H42), C43(H43), C44(H44), C45(H45), C46(H46)
2.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              25288
_shelx_fab_checksum              54441
_olex2_date_sample_data_collection 2020-05-28
_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 1.361
_oxdiff_exptl_absorpt_empirical_full_min 0.800