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_7703034
_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         'C53 H58 N2 P2'
_chemical_formula_sum            'C53 H58 N2 P2'
_chemical_formula_weight         784.95
_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     dual
_audit_creation_date             2018-02-19
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-09-26 deposited with the CCDC.	2019-12-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.226(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.6214(12)
_cell_length_b                   10.9205(5)
_cell_length_c                   20.4742(10)
_cell_measurement_reflns_used    12333
_cell_measurement_temperature    120.03(10)
_cell_measurement_theta_max      27.4670
_cell_measurement_theta_min      2.6980
_cell_volume                     4686.0(4)
_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      120.03(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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     65.00  91.00   1.00  120.62    --   10.50  77.00  90.00   26
  2  \w    -62.00  39.00   1.00  120.62    --   10.50 -57.00 120.00  101
  3  \w     63.00  89.00   1.00  120.62    --   10.50  57.00-150.00   26
  4  \w     64.00  94.00   1.00  120.62    --   10.50  77.00-180.00   30
  5  \w    -46.00  38.00   1.00  120.62    --   10.50 -82.00-120.00   84
  6  \w     58.00  90.00   1.00  120.62    --   10.50  77.00 -60.00   32
  7  \w     51.00  81.00   1.00  120.62    --   10.50  77.00   0.00   30
  8  \w    -55.00 -29.00   1.00  120.62    --  -10.90 -82.00   0.00   26
  9  \w    -15.00  32.00   1.00  120.62    --  -10.90 -82.00-150.00   47
 10  \w      7.00  32.00   1.00  120.62    --  -10.90 -82.00 -60.00   25
 11  \w    -41.00  15.00   1.00  120.62    --  -10.90 -82.00 120.00   56
 12  \w    -60.00 -20.00   1.00  120.62    --  -10.90 -82.00  30.00   40
 13  \w    -48.00 -23.00   1.00  120.62    --  -10.90 -77.00-180.00   25
 14  \w    -18.00  26.00   1.00  120.62    --  -10.90 -82.00   0.00   44
 15  \w    -59.00 -20.00   1.00  120.62    --  -10.90 -82.00 -60.00   39
;
_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      -0.0016339000
_diffrn_orient_matrix_UB_12      -0.0081765000
_diffrn_orient_matrix_UB_13      -0.0347561000
_diffrn_orient_matrix_UB_21      0.0305604000
_diffrn_orient_matrix_UB_22      -0.0278763000
_diffrn_orient_matrix_UB_23      0.0082980000
_diffrn_orient_matrix_UB_31      -0.0144201000
_diffrn_orient_matrix_UB_32      -0.0580956000
_diffrn_orient_matrix_UB_33      0.0009162000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0680
_diffrn_reflns_av_unetI/netI     0.0536
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            64797
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.498
_diffrn_reflns_theta_min         2.694
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.128
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68808
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.113
_exptl_crystal_description       needle
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.407
_exptl_crystal_size_mid          0.131
_exptl_crystal_size_min          0.119
_refine_diff_density_max         0.333
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     528
_refine_ls_number_reflns         9713
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0825
_refine_ls_R_factor_gt           0.0627
_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^)+(0.0483P)^2^+5.3343P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1323
_refine_ls_wR_factor_ref         0.1396
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7639
_reflns_number_total             9713
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04690a2.cif
_cod_data_source_block           aj0190
_cod_depositor_comments
'Adding full bibliography for 7703034--7703036.cif.'
_cod_database_code               7703034
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C48 H50 N2 P1'
_reflns_odcompleteness_completeness 99.84
_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 Aromatic/amide H refined with riding coordinates:
 C25(H25), C8(H8), C10(H10), C38(H38), C9(H9), C34(H34), C40(H40), C16(H16),
 C23(H23), C32(H32), C49(H49), C33(H33), C14(H14), C47(H47), C3(H3), C2(H2)
2.b Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C27(H27A,H27B,H27C), C19(H19A,H19B,H19C), C44(H44A,H44B,
 H44C), C53(H53A,H53B,H53C), C43(H43A,H43B,H43C), C4(H4A,H4B,H4C), C18(H18A,
 H18B,H18C), C5(H5A,H5B,H5C), C42(H42A,H42B,H42C), C28(H28A,H28B,H28C),
 C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              63831
_shelx_fab_checksum              41188
_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 1.386
_oxdiff_exptl_absorpt_empirical_full_min 0.580