Improved reactivity of a cyclic 13/15 compound by increased steric demand
Balmer, Markus; Kapitein, Manuel; von Hänisch, Carsten; Dalton Trans.  (2017) –; doi:10.1039/C7DT00950J

data_7043042
_publ_section_title
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 Improved reactivity of a cyclic 13/15 compound by increased steric demand
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT00950J
_journal_year                    2017
_chemical_formula_moiety         'C31 H49 Ga N2 P Si'
_chemical_formula_sum            'C31 H49 Ga N2 P Si'
_chemical_formula_weight         578.50
_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     dual
_audit_creation_date             2017-02-22
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2017-02-23 deposited with the CCDC.
2017-05-01 downloaded from the CCDC.
;
_cell_angle_alpha                75.424(2)
_cell_angle_beta                 87.916(2)
_cell_angle_gamma                69.400(2)
_cell_formula_units_Z            2
_cell_length_a                   9.9548(5)
_cell_length_b                   12.7363(6)
_cell_length_c                   14.9374(7)
_cell_measurement_reflns_used    9929
_cell_measurement_temperature    240.0
_cell_measurement_theta_max      25.297
_cell_measurement_theta_min      2.189
_cell_volume                     1712.87(15)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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      240.0
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23472
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.304
_diffrn_reflns_theta_min         1.767
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.904
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6893
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0908 before and 0.0431 after correction. The Ratio of minimum to maximum transmission is 0.9250. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.122
_exptl_crystal_description       block
_exptl_crystal_F_000             618
_exptl_crystal_size_max          0.392
_exptl_crystal_size_mid          0.375
_exptl_crystal_size_min          0.228
_refine_diff_density_max         0.679
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         6228
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0371
_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^)+(0.0535P)^2^+1.2618P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0978
_refine_ls_wR_factor_ref         0.1029
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5337
_reflns_number_total             6228
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00950j2.cif
_cod_data_source_block           compound2
_cod_database_code               7043042
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H) groups, All C(H,H,H) groups
2. Others
 1*[Sof(C15)+Sof(C16)+Sof(C17)]+1*[Sof(C15A)+Sof(C16A)+Sof(C17A)]+1*[Sof(C17B)+
 Sof(C15B)+Sof(C16B)]=1 with esd of 0.0001
 Sof(C15)=Sof(C16)=Sof(C17)=FVAR(1)
 Sof(C15A)=Sof(C16A)=Sof(C17A)=FVAR(2)
 Sof(C17B)=Sof(C15B)=Sof(C16B)=FVAR(3)
3.a Ternary CH refined with riding coordinates:
 C4(H4), C7(H7)
3.b Aromatic/amide H refined with riding coordinates:
 C27(H27), C28(H28), C29(H29), C30(H30), C31(H31)
3.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C12(H12A,
 H12B,H12C), C13(H13A,H13B,H13C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C),
 C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C)
;
_olex2_submission_special_instructions 'No special instructions were received'