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_7703035
_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         'C48 H51 O P2, C7 H13 N2'
_chemical_formula_sum            'C55 H64 N2 O P2'
_chemical_formula_weight         831.02
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-08-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-10-01 deposited with the CCDC.	2019-12-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.797(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.7505(7)
_cell_length_b                   16.1364(8)
_cell_length_c                   18.1430(8)
_cell_measurement_reflns_used    6784
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      29.0880
_cell_measurement_theta_min      2.7070
_cell_volume                     4846.2(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_temperature      120.01(10)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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     11.00  36.00   0.50   48.14    --    7.10  65.00-162.00   50
  2  \w    -46.00 -21.00   0.50   48.14    --    7.10 -65.00  61.00   50
  3  \w     -3.00  22.00   0.50   48.14    --   -7.50  65.00-162.00   50
  4  \w    -44.00 -19.00   0.50   48.14    --   -7.50 -65.00  61.00   50
  5  \w     50.00  93.00   0.50   48.14    --    7.10  77.00 120.00   86
  6  \w     60.00  92.00   0.50   48.14    --    7.10  77.00  30.00   64
  7  \w     50.00  96.00   0.50   48.14    --    7.10  77.00 -30.00   92
  8  \w     58.00  93.00   0.50   48.14    --    7.10  77.00 -90.00   70
  9  \w     56.00  82.00   0.50   48.14    --    7.10  77.00-120.00   52
 10  \w     54.00  90.00   0.50   48.14    --    7.10  77.00  60.00   72
 11  \w    -50.00  -8.00   0.50   48.14    --   -7.50 -82.00 150.00   84
 12  \w    -72.00 -30.00   0.50   48.14    --   -7.50 -57.00-120.00   84
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0506
_diffrn_reflns_av_unetI/netI     0.0599
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            23911
_diffrn_reflns_point_group_measured_fraction_full 0.901
_diffrn_reflns_point_group_measured_fraction_max 0.901
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.723
_exptl_absorpt_coefficient_mu    0.129
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.32893
_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    1.139
_exptl_crystal_description       block
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.176
_exptl_crystal_size_min          0.128
_refine_diff_density_max         0.173
_refine_diff_density_min         -0.204
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details
;
 Flack x determined using 2524 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.04(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         7694
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0374
_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^)+(0.0425P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0805
_refine_ls_wR_factor_ref         0.0837
_reflns_Friedel_coverage         0.804
_reflns_Friedel_fraction_full    0.804
_reflns_Friedel_fraction_max     0.804
_reflns_number_gt                6684
_reflns_number_total             7694
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04690a2.cif
_cod_data_source_block           aj0189
_cod_depositor_comments
'Adding full bibliography for 7703034--7703036.cif.'
_cod_database_code               7703035
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.984
_shelx_estimated_absorpt_t_min   0.971
_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:
 C5(H5)
2.b Aromatic/amide H refined with riding coordinates:
 C27(H27), C1(H1A), C42(H42), C40(H40), C25(H25), C16(H16), C11(H11), C12(H12),
  C10(H10), C34(H34), C2(H2), C48(H48), C36(H36), C50(H50), C3(H3), C35(H35),
 C18(H18)
2.c Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C43(H43A,H43B,H43C), C29(H29A,H29B,H29C), C4(H4A,H4B,
 H4C), C20(H20A,H20B,H20C), C45(H45A,H45B,H45C), C22(H22A,H22B,H22C), C54(H54A,
 H54B,H54C), C53(H53A,H53B,H53C), C52(H52A,H52B,H52C), C44(H44A,H44B,H44C),
 C31(H31A,H31B,H31C), C21(H21A,H21B,H21C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C)
;
_shelx_res_checksum              11213
_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
;