Reactivity enhancement of a diphosphene by reversible N-heterocyclic carbene coordination.
Dhara, Debabrata; Kalita, Pankaj; Mondal, Subhadip; Narayanan, Ramakirushnan Suriya; Mote, Kaustubh R.; Huch, Volker; Zimmer, Michael; Yildiz, Cem B.; Scheschkewitz, David; Chandrasekhar, Vadapalli; Jana, Anukul; Chemical science 9 (2018) 4235–4243; doi:10.1039/c8sc00348c

data_1549138
_publ_section_title
;
 Reactivity enhancement of a diphosphene by reversible N-heterocyclic
 carbene coordination.
;
_journal_issue                   18
_journal_name_full               'Chemical science'
_journal_page_first              4235
_journal_page_last               4243
_journal_paper_doi               10.1039/c8sc00348c
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         'C48 H52 O P2'
_chemical_formula_sum            'C48 H52 O P2'
_chemical_formula_weight         706.83
_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'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-11-06
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-11-30 deposited with the CCDC.
2018-03-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.9466(7)
_cell_length_b                   20.6986(9)
_cell_length_c                   23.0289(10)
_cell_measurement_reflns_used    9895
_cell_measurement_temperature    151.25
_cell_measurement_theta_max      25.83
_cell_measurement_theta_min      2.35
_cell_volume                     8077.9(6)
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      151.25
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0620
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            139724
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.974
_diffrn_reflns_theta_min         1.769
_exptl_absorpt_coefficient_mu    0.142
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7181
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_description       block
_exptl_crystal_F_000             3024
_exptl_crystal_size_max          0.442
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.154
_refine_diff_density_max         0.944
_refine_diff_density_min         -0.553
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         9733
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0822
_refine_ls_R_factor_gt           0.0616
_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^)+(0.0793P)^2^+10.4981P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1624
_refine_ls_wR_factor_ref         0.1791
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7481
_reflns_number_total             9733
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc00348c2.cif
_cod_data_source_block           sh3914
_cod_depositor_comments
'Adding full bibliography for 1549135--1549139.cif.'
_cod_database_code               1549138
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.978
_shelx_estimated_absorpt_t_min   0.940
_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:
 C27(H27), C28(H28), C29(H29), C35(H35), C33(H33), C42(H42), C44(H44), C5(H5),
 C4(H4), C3(H3), C20(H20), C18(H18), C11(H11), C9(H9)
2.b Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C38(H38A,H38B,H38C), C37(H37A,H37B,H37C), C46(H46A,H46B,
 H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C24(H24A,H24B,H24C), C23(H23A,
 H23B,H23C), C22(H22A,H22B,H22C), C15(H15A,H15B,H15C), C14(H14A,H14B,H14C),
 C13(H13A,H13B,H13C)
;
_shelx_res_checksum              63251
_olex2_submission_special_instructions 'No special instructions were received'