An NHC‒phosphinidenyl as a synthon for new group 13/15 compounds
Lemp, Otfried; Balmer, Markus; Reiter, Kevin; Weigend, Florian; von Hänisch, Carsten; Chem. Commun.  (2017) –; doi:10.1039/C7CC04422D

data_7120321
_publ_section_title
;
 An NHC--phosphinidenyl as a synthon for new group 13/15 compounds
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC04422D
_journal_year                    2017
_chemical_formula_moiety         'C29 H45 Al Cl N2 P'
_chemical_formula_sum            'C29 H45 Al Cl N2 P'
_chemical_formula_weight         515.07
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-03-15
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-03-10 deposited with the CCDC.
2017-06-15 downloaded from the CCDC.
;
_cell_angle_alpha                83.758(2)
_cell_angle_beta                 87.788(2)
_cell_angle_gamma                68.557(2)
_cell_formula_units_Z            2
_cell_length_a                   9.6040(6)
_cell_length_b                   10.8306(7)
_cell_length_c                   16.4507(10)
_cell_measurement_reflns_used    8603
_cell_measurement_temperature    115(2)
_cell_measurement_theta_max      27.442
_cell_measurement_theta_min      2.272
_cell_volume                     1583.27(17)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      114.99
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_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  0.0869
_diffrn_reflns_av_unetI/netI     0.0840
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            32732
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.601
_diffrn_reflns_theta_min         2.272
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.217
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6615
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1441 before and 0.0553 after correction.
The Ratio of minimum to maximum transmission is 0.8872.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.080
_exptl_crystal_description       block
_exptl_crystal_F_000             556
_exptl_crystal_size_max          0.494
_exptl_crystal_size_mid          0.436
_exptl_crystal_size_min          0.224
_refine_diff_density_max         0.358
_refine_diff_density_min         -0.272
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         7290
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.1094
_refine_ls_R_factor_gt           0.0610
_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^)+(0.0510P)^2^+1.0430P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1204
_refine_ls_wR_factor_ref         0.1316
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4787
_reflns_number_total             7290
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc04422d2.cif
_cod_data_source_block           pm34_0m
_cod_database_code               7120321
_shelx_estimated_absorpt_t_max   0.953
_shelx_estimated_absorpt_t_min   0.900
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B)
2.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C6(H6), C15(H15), C17(H17)
2.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C25(H25A,H25B,H25C), C11(H11A,H11B,
 H11C), C24(H24A,H24B,H24C), C19(H19A,H19B,H19C), C27(H27A,H27B,H27C), C23(H23A,
 H23B,H23C), C29(H29A,H29B,H29C), C28(H28A,H28B,H28C), C21(H21A,H21B,H21C),
 C20(H20A,H20B,H20C)
;
_shelx_res_checksum              16595
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'