N-Heterocyclic carbene phosphaketene adducts as precursors to carbene-phosphinidene adducts and a rearranged π-system.
Li, Zhongshu; Chen, Xiaodan; Li, Yaqi; Su, Cheng-Yong; Grützmacher, Hansjörg; Chemical communications (Cambridge, England) 52 (2016) 11343–11346; doi:10.1039/c6cc05916c

data_7124964
_publ_section_title
;
 N-Heterocyclic carbene phosphaketene adducts as precursors to
 carbene-phosphinidene adducts and a rearranged \p-system.
;
_journal_issue                   76
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              11343
_journal_page_last               11346
_journal_paper_doi               10.1039/c6cc05916c
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C46 H51 N2 O P Sn'
_chemical_formula_sum            'C46 H51 N2 O P Sn'
_chemical_formula_weight         797.54
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-07-02
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-03-18 deposited with the CCDC.
2016-08-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.185(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0166(3)
_cell_length_b                   19.8309(6)
_cell_length_c                   14.9450(4)
_cell_measurement_reflns_used    10386
_cell_measurement_temperature    100
_cell_measurement_theta_max      65.3490
_cell_measurement_theta_min      4.3470
_cell_volume                     4143.06(19)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_unetI/netI     0.0492
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.906
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            40641
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.906
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.654
_diffrn_reflns_theta_min         2.814
_exptl_absorpt_coefficient_mu    0.691
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_description       block
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.018
_refine_diff_density_max         1.361
_refine_diff_density_min         -0.768
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     653
_refine_ls_number_reflns         13762
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0442
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0253P)^2^+2.4179P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0796
_refine_ls_wR_factor_ref         0.0851
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11320
_reflns_number_total             13762
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc05916c2.cif
_cod_data_source_block           exp_2625
_cod_original_cell_volume        4143.07(19)
_cod_database_code               7124964
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C)
;
_olex2_date_sample_data_collection 2015-06-27
_olex2_submission_special_instructions 'No special instructions were received'