Isolable N-heterocyclic carbene adducts of the elusive diiodophosphine.
Cicač-Hudi, M; Schlindwein, S. H.; Feil, C. M.; Nieger, M.; Gudat, D.; Chemical communications (Cambridge, England) 54 (2018) 7645–7648; doi:10.1039/c8cc03972k

data_7121872
_publ_section_title
;
 Isolable N-heterocyclic carbene adducts of the elusive diiodophosphine.
;
_journal_issue                   55
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              7645
_journal_page_last               7648
_journal_paper_doi               10.1039/c8cc03972k
_journal_volume                  54
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C21 H25 I2 N2 P'
_chemical_formula_sum            'C21 H25 I2 N2 P'
_chemical_formula_weight         590.20
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-05-11 deposited with the CCDC.
2018-06-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2530(6)
_cell_length_b                   15.3097(11)
_cell_length_c                   16.0029(13)
_cell_measurement_reflns_used    4640
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      28.1
_cell_measurement_theta_min      1.8
_cell_volume                     2267.0(3)
_computing_cell_refinement       'Bruker ApexII Software Suite, 2008'
_computing_data_collection       'Bruker ApexII Software Suite, 2008'
_computing_data_reduction        'Bruker ApexII Software Suite, 2008'
_computing_molecular_graphics    'SHELXS plus XP (Sheldrick, 1991)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Kappa ApexII Duo'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_unetI/netI     0.0543
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20732
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.182
_diffrn_reflns_theta_min         1.841
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.852
_exptl_absorpt_correction_T_max  0.6920
_exptl_absorpt_correction_T_min  0.5513
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.729
_exptl_crystal_description       prism
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.215
_exptl_crystal_size_mid          0.194
_exptl_crystal_size_min          0.154
_refine_diff_density_max         0.804
_refine_diff_density_min         -0.854
_refine_diff_density_rms         0.106
_refine_ls_abs_structure_details
;
 Flack x determined using 1751 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.034(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         5584
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0342
_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^)+(0.0260P)^2^+0.3721P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0601
_refine_ls_wR_factor_ref         0.0651
_reflns_Friedel_coverage         0.773
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                4639
_reflns_number_total             5584
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc03972k2.cif
_cod_data_source_block           g407_mn
_cod_depositor_comments
'Adding full bibliography for 7121868--7121873.cif.'
_cod_database_code               7121872
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.579
_shelx_estimated_absorpt_t_max   0.668
_shelx_res_checksum              44971