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_1549139
_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 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           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   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                 93.710(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.2280(18)
_cell_length_b                   16.3739(19)
_cell_length_c                   17.6769(19)
_cell_measurement_reflns_used    4995
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.63
_cell_measurement_theta_min      2.15
_cell_volume                     4687.2(9)
_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 2014/5 (Sheldrick, 2014)'
_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 1.000
_diffrn_measured_fraction_theta_max 0.996
_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  0.1256
_diffrn_reflns_av_unetI/netI     0.0828
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            50415
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.422
_diffrn_reflns_theta_min         1.651
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.133
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6074
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0790 before and 0.0645 after correction.
The Ratio of minimum to maximum transmission is 0.8151.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_description       block
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.347
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     561
_refine_ls_number_reflns         8602
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1117
_refine_ls_R_factor_gt           0.0549
_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^)+(0.0530P)^2^+3.7877P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1173
_refine_ls_wR_factor_ref         0.1454
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5295
_reflns_number_total             8602
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc00348c2.cif
_cod_data_source_block           vc_aj_slnf
_cod_depositor_comments
'Adding full bibliography for 1549135--1549139.cif.'
_cod_database_code               1549139
_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:
 C40(H40), C42(H42), C12(H12), C34(H34), C18(H18), C11(H11), C51(H51),
 C36(H36), C10(H10), C27(H27), C16(H16), C25(H25), C49(H49), C35(H35), C1(H1C)
2.b Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C22(H22A,H22B,H22C), C29(H29A,H29B,H29C), C20(H20A,H20B,
 H20C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C31(H31A,H31B,H31C), C54(H54A,
 H54B,H54C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C53(H53A,H53B,
 H53C), C55(H55A,H55B,H55C), C7(H7A,H7B,H7C), C21(H21A,H21B,H21C), C30(H30A,
 H30B,H30C)
;
_shelx_res_checksum              44970
_olex2_submission_special_instructions 'No special instructions were received'