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_1549135
_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         'C55 H62 N2 P2'
_chemical_formula_sum            'C55 H62 N2 P2'
_chemical_formula_weight         813.00
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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                 97.766(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9502(8)
_cell_length_b                   20.9614(14)
_cell_length_c                   20.7528(17)
_cell_measurement_reflns_used    5671
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.56
_cell_measurement_theta_min      2.22
_cell_volume                     4719.7(6)
_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      100(2)
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2318
_diffrn_reflns_av_unetI/netI     0.1293
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            58867
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.672
_diffrn_reflns_theta_min         1.387
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.130
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5594
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1391 before and 0.0723 after correction. The Ratio of minimum to maximum transmission is 0.7507. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.144
_exptl_crystal_description       block
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.523
_refine_diff_density_min         -0.416
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     548
_refine_ls_number_reflns         8812
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1814
_refine_ls_R_factor_gt           0.1016
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1319P)^2^+11.6372P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2418
_refine_ls_wR_factor_ref         0.3141
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4613
_reflns_number_total             8812
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc00348c2.cif
_cod_data_source_block           vc_aj_180617
_cod_depositor_comments
'Adding full bibliography for 1549135--1549139.cif.'
_cod_database_code               1549135
_shelx_shelxl_version_number     2017/1
_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:
 C18(H18), C16(H16), C27(H27), C25(H25), C34(H34), C36(H36), C35(H35),
 C49(H49), C10(H10), C51(H51), C42(H42), C12(H12), C11(H11), C40(H40)
2.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C31(H31A,H31B,H31C), C53(H53A,H53B,H53C), C20(H20A,H20B,
 H20C), C55(H55A,H55B,H55C), C22(H22A,H22B,H22C), C29(H29A,H29B,H29C), C30(H30A,
 H30B,H30C), C46(H46A,H46B,H46C), C6(H6A,H6B,H6C), C21(H21A,H21B,H21C), C4(H4A,
 H4B,H4C), C44(H44A,H44B,H44C), C7(H7A,H7B,H7C), C54(H54A,H54B,H54C), C45(H45A,
 H45B,H45C)
;
_shelx_res_checksum              92913
_olex2_submission_special_instructions 'No special instructions were received'