Influence of N-heterocyclic carbenes (NHCs) on the hydrolysis of a diphosphene.
Dhara, Debabrata; Das, Shubhajit; Kalita, Pankaj; Maiti, Avijit; Pati, Swapan K.; Scheschkewitz, David; Chandrasekhar, Vadapalli; Jana, Anukul; Dalton transactions (Cambridge, England : 2003) 49 (2020) 993–997; doi:10.1039/c9dt04690a

data_7703036
_publ_section_title
;
 Influence of N-heterocyclic carbenes (NHCs) on the hydrolysis of a
 diphosphene.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              993
_journal_page_last               997
_journal_paper_doi               10.1039/c9dt04690a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety
'2(C48 H51 O P2), C11 H21 N2, C11 H20 N2, 2(C7 H8)'
_chemical_formula_sum            'C132 H159 N4 O2 P4'
_chemical_formula_weight         1957.50
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-12-05
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-09-30 deposited with the CCDC.	2019-12-23 downloaded from the CCDC.
;
_cell_angle_alpha                66.943(5)
_cell_angle_beta                 81.227(4)
_cell_angle_gamma                81.959(4)
_cell_formula_units_Z            2
_cell_length_a                   12.9095(6)
_cell_length_b                   21.2248(12)
_cell_length_c                   23.3462(11)
_cell_measurement_reflns_used    12906
_cell_measurement_temperature    293.12(10)
_cell_measurement_theta_max      27.8420
_cell_measurement_theta_min      2.7520
_cell_volume                     5794.4(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_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      293.12(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_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    -43.00  -2.00   1.00  103.67    --    3.30 -38.00-150.00   41
  2  \w    -63.00 -26.00   1.00  103.67    --    3.30 -82.00 150.00   37
  3  \w     -7.00  20.00   1.00  103.67    --    3.30 -82.00 150.00   27
  4  \w     -6.00  20.00   1.00  103.67    --    3.30  57.00  90.00   26
  5  \w     53.00  86.00   1.00  103.67    --   -3.60  57.00 150.00   33
  6  \w    -93.00  27.00   1.00  103.67    --   -3.60 -57.00  60.00  120
  7  \w    -63.00  19.00   1.00  103.67    --   -3.60 -82.00-150.00   82
  8  \w    -60.00 -35.00   1.00  103.67    --   -3.60 -82.00   0.00   25
  9  \w    -16.00  22.00   1.00  103.67    --   -3.60 -38.00 -30.00   38
 10  \w    -37.00  -9.00   1.00  103.67    --   -3.60 -82.00 120.00   28
 11  \w    -59.00 -33.00   1.00  103.67    --   -3.60 -82.00 -60.00   26
 12  \w    -87.00  24.00   1.00  103.67    --   -3.60 -38.00-120.00  111
 13  \w    -92.00 -39.00   1.00  103.67    --   -3.60 -38.00 -30.00   53
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0357392000
_diffrn_orient_matrix_UB_12      -0.0179172000
_diffrn_orient_matrix_UB_13      0.0225632000
_diffrn_orient_matrix_UB_21      -0.0393264000
_diffrn_orient_matrix_UB_22      0.0020274000
_diffrn_orient_matrix_UB_23      0.0241522000
_diffrn_orient_matrix_UB_31      -0.0170618000
_diffrn_orient_matrix_UB_32      -0.0316909000
_diffrn_orient_matrix_UB_33      0.0032476000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0829
_diffrn_reflns_av_unetI/netI     0.0680
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            120222
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.500
_diffrn_reflns_theta_min         2.522
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.117
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.33767
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.122
_exptl_crystal_description       needle
_exptl_crystal_F_000             2110
_exptl_crystal_size_max          0.602
_exptl_crystal_size_mid          0.097
_exptl_crystal_size_min          0.078
_refine_diff_density_max         1.206
_refine_diff_density_min         -0.729
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1325
_refine_ls_number_reflns         23931
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0945
_refine_ls_R_factor_gt           0.0575
_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^)+(0.0613P)^2^+3.4300P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1325
_refine_ls_wR_factor_ref         0.1483
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16245
_reflns_number_total             23931
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04690a2.cif
_cod_data_source_block           aj0093
_cod_depositor_comments
'Adding full bibliography for 7703034--7703036.cif.'
_cod_database_code               7703036
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C66 H68 N2 O P2'
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C9A(H9A), C4A(H4A), C9B(H9B)
2.b Aromatic/amide H refined with riding coordinates:
 C14B(H14B), C1A(H1AA), C29A(H29A), C16B(H16B), C16A(H16A), C15B(H15B),
 C14A(H14A), C31A(H31A), C31B(H31B), C53B(H53B), C55A(H55A), C22A(H22A),
 C53A(H53A), C15A(H15A), C20B(H20B), C29B(H29B), C40A(H40A), C44A(H44A),
 C38B(H38B), C55B(H55B), C20A(H20A), C40B(H40B), C46A(H46A), C38A(H38A),
 C39A(H39A), C22B(H22B), C39B(H39B), C46B(H46B), C44B(H44B), C1B(H1BA),
 C61A(H61A), C62A(H62A), C65A(H65A), C65B(H65B), C63A(H63A), C61B(H61B),
 C64B(H64B), C64A(H64A), C62B(H62B), C63B(H63B)
2.c Idealised Me refined as rotating group:
 C24B(H24D,H24E,H24F), C26A(H26A,H26B,H26C), C35A(H35A,H35B,H35C), C6A(H6AA,
 H6AB,H6AC), C33A(H33A,H33B,H33C), C26B(H26D,H26E,H26F), C57A(H57A,H57B,H57C),
 C35B(H35D,H35E,H35F), C57B(H57D,H57E,H57F), C50B(H50D,H50E,H50F), C59B(H59D,
 H59E,H59F), C48A(H48A,H48B,H48C), C10A(H10A,H10B,H10C), C50A(H50A,H50B,H50C),
 C5A(H5AA,H5AB,H5AC), C34B(H34D,H34E,H34F), C24A(H24A,H24B,H24C), C11A(H11A,
 H11B,H11C), C58A(H58A,H58B,H58C), C59A(H59A,H59B,H59C), C33B(H33D,H33E,H33F),
 C34A(H34A,H34B,H34C), C49A(H49A,H49B,H49C), C8B(H8BA,H8BB,H8BC), C58B(H58D,
 H58E,H58F), C7A(H7AA,H7AB,H7AC), C48B(H48D,H48E,H48F), C8A(H8AA,H8AB,H8AC),
 C25B(H25D,H25E,H25F), C6B(H6BA,H6BB,H6BC), C49B(H49D,H49E,H49F), C7B(H7BA,H7BB,
 H7BC), C25A(H25A,H25B,H25C), C66A(H66A,H66B,H66C), C10B(H10D,H10E,H10F),
 C5B(H5BA,H5BB,H5BC), C11B(H11D,H11E,H11F), C66B(H66D,H66E,H66F)
;
_shelx_res_checksum              13733
_shelx_fab_checksum              94959
_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 1.810
_oxdiff_exptl_absorpt_empirical_full_min 0.339