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_7710159
_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         'C46 H51 N2 P'
_chemical_formula_sum            'C46 H51 N2 P'
_chemical_formula_weight         662.85
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2020-04-30
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.2225(4)
_cell_length_b                   18.7068(4)
_cell_length_c                   20.3020(4)
_cell_measurement_reflns_used    33994
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      31.9070
_cell_measurement_theta_min      2.6950
_cell_volume                     7680.2(3)
_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      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.965
_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   44.00    --  -17.08 -77.00 -60.00   55
  2  \w     -8.00  85.00   1.00   44.00    --   17.08  57.00-150.00   93
  3  \w     -4.00  88.00   1.00   44.00    --   17.08  38.00 120.00   92
  4  \w      3.00  88.00   1.00   44.00    --   17.08  38.00 -60.00   85
  5  \w    -59.00  50.00   1.00   44.00    --   17.08 -19.00 120.00  109
  6  \w      0.00  67.00   1.00   44.00    --   17.08-118.00 -69.97   67
  7  \w      0.00  67.00   1.00   44.00    --   17.08-118.00 113.80   67
  8  \w    -51.00  42.00   1.00   44.00    --   17.08 -57.00 -30.00   93
  9  \w     55.00  70.00   1.00   44.00    --   17.08-154.00-153.27   15
;
_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      0.0261836000
_diffrn_orient_matrix_UB_12      -0.0237001000
_diffrn_orient_matrix_UB_13      0.0079034000
_diffrn_orient_matrix_UB_21      -0.0230048000
_diffrn_orient_matrix_UB_22      -0.0240505000
_diffrn_orient_matrix_UB_23      0.0143514000
_diffrn_orient_matrix_UB_31      -0.0039897000
_diffrn_orient_matrix_UB_32      -0.0172419000
_diffrn_orient_matrix_UB_33      -0.0308554000
_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  0.0622
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            162835
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.877
_diffrn_reflns_theta_min         2.495
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.105
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.574
_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            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.147
_exptl_crystal_description       plate
_exptl_crystal_F_000             2848
_exptl_crystal_size_max          0.309
_exptl_crystal_size_mid          0.246
_exptl_crystal_size_min          0.098
_refine_diff_density_max         0.419
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     646
_refine_ls_number_reflns         13820
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0492
_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^)+(0.0530P)^2^+3.4464P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1133
_refine_ls_wR_factor_ref         0.1262
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10265
_reflns_number_total             13820
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01314b2.cif
_cod_data_source_block           compound_4a
_cod_database_code               7710159
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C46H51N2P
_shelx_estimated_absorpt_t_max   0.990
_shelx_estimated_absorpt_t_min   0.968
_diffrn_oxdiff_digest_frames
;
012bd8b2837bb5e2a7a4d47768f1240adf00676aff0
;
_diffrn_oxdiff_digest_hkl
;
0123dbb7f06d5dc2e8c0e39f26e67b03830f38
;
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.97
_olex2_refinement_description
;
;
_shelx_res_checksum              89088
_olex2_date_sample_data_collection 2020-04-16
_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 1.140
_oxdiff_exptl_absorpt_empirical_full_min 0.954