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_7043041
_publ_section_title
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 Improved reactivity of a cyclic 13/15 compound by increased steric demand
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_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT00950J
_journal_year                    2017
_chemical_formula_moiety         'C43 H66 Ga N2 P Si'
_chemical_formula_sum            'C43 H66 Ga N2 P Si'
_chemical_formula_weight         739.75
_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             2017-01-25
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
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2017-02-23 deposited with the CCDC.
2017-05-01 downloaded from the CCDC.
;
_cell_angle_alpha                94.041(1)
_cell_angle_beta                 91.976(2)
_cell_angle_gamma                105.366(2)
_cell_formula_units_Z            8
_cell_length_a                   18.7845(7)
_cell_length_b                   22.0925(9)
_cell_length_c                   26.3432(11)
_cell_measurement_reflns_used    9566
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      28.333
_cell_measurement_theta_min      2.346
_cell_volume                     10499.3(7)
_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      100.0
_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 0.996
_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  0.0652
_diffrn_reflns_av_unetI/netI     0.0516
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            340992
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.368
_diffrn_reflns_theta_min         2.177
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.602
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6753
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1561 before and 0.0530 after correction. The Ratio of minimum to maximum transmission is 0.9056. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.936
_exptl_crystal_description       block
_exptl_crystal_F_000             3184
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.098
_refine_diff_density_min         -0.677
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1959
_refine_ls_number_reflns         52367
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0433
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0440P)^2^+4.7490P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0925
_refine_ls_wR_factor_ref         0.1005
_reflns_Friedel_coverage         0.000
_reflns_number_gt                38179
_reflns_number_total             52367
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00950j2.cif
_cod_data_source_block           compound3
_cod_database_code               7043041
_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,H) groups
2. Rigid bond restraints
 C175, C181, C176, C182, C177, C202, C183, C184, C179, C185, C180, C186
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C0BA, C168
 with sigma for 1-2 distances of 106 and sigma for 1-3 distances of 206
3. Others
 Sof(C181)=Sof(C182)=Sof(H182)=Sof(C202)=Sof(H202)=Sof(C184)=Sof(H184)=
 Sof(C185)=Sof(H185)=Sof(C186)=Sof(H186)=Sof(C160)=Sof(C161)=Sof(H16J)=
 Sof(H16K)=Sof(H16L)=Sof(C162)=Sof(H16M)=Sof(H16N)=Sof(H16O)=Sof(C169)=
 Sof(H16P)=Sof(H16Q)=Sof(H16R)=Sof(C163)=Sof(H16S)=Sof(H16T)=Sof(H16U)=
 Sof(C171)=Sof(H17J)=Sof(H17K)=Sof(H17L)=Sof(C168)=Sof(C170)=Sof(H17M)=
 Sof(H17N)=Sof(H17O)=Sof(Si4B)=1-FVAR(1)
 Sof(C175)=Sof(C176)=Sof(H176)=Sof(C177)=Sof(H177)=Sof(C183)=Sof(H183)=
 Sof(C179)=Sof(H179)=Sof(C180)=Sof(H180)=Sof(C164)=Sof(C165)=Sof(H16A)=
 Sof(H16B)=Sof(H16C)=Sof(C166)=Sof(H16D)=Sof(H16E)=Sof(H16F)=Sof(C167)=
 Sof(H16G)=Sof(H16H)=Sof(H16I)=Sof(C0BA)=Sof(C172)=Sof(H17A)=Sof(H17B)=
 Sof(H17C)=Sof(C173)=Sof(H17D)=Sof(H17E)=Sof(H17F)=Sof(C174)=Sof(H17G)=
 Sof(H17H)=Sof(H17I)=Sof(Si4A)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C132(H132), C88(H88), C144(H144), C45(H45), C3(H3A), C131(H131), C58(H58),
 C46(H46), C2(H2A), C103(H103), C86(H86), C125(H125), C137(H137), C82(H82),
 C39(H39), C6(H6), C51(H51), C127(H127), C92(H92), C126(H126), C15(H15),
 C85(H85), C84(H84), C41(H41), C129(H129), C89(H89), C147(H147), C135(H135),
 C60(H60), C128(H128), C43(H43), C94(H94), C49(H49), C17(H17), C101(H101),
 C8(H8), C83(H83), C40(H40), C42(H42), C176(H176), C177(H177), C183(H183),
 C179(H179), C180(H180), C182(H182), C202(H202), C184(H184), C185(H185),
 C186(H186)
4.b Idealised Me refined as rotating group:
 C107(H10A,H10B,H10C), C53(H53A,H53B,H53C), C32(H32A,H32B,H32C), C98(H98A,H98B,
 H98C), C66(H66A,H66B,H66C), C64(H64A,H64B,H64C), C10(H10M,H10N,H10O),
 C122(H12A,H12B,H12C), C36(H36A,H36B,H36C), C62(H62A,H62B,H62C), C139(H13A,H13B,
 H13C), C151(H15A,H15B,H15C), C121(H12D,H12E,H12F), C96(H96A,H96B,H96C),
 C118(H11A,H11B,H11C), C33(H33A,H33B,H33C), C159(H15D,H15E,H15F), C117(H11D,
 H11E,H11F), C28(H28A,H28B,H28C), C149(H14A,H14B,H14C), C123(H12G,H12H,H12I),
 C37(H37A,H37B,H37C), C79(H79A,H79B,H79C), C78(H78A,H78B,H78C), C119(H11G,H11H,
 H11I), C105(H10D,H10E,H10F), C35(H35A,H35B,H35C), C27(H27A,H27B,H27C),
 C24(H24A,H24B,H24C), C67(H67A,H67B,H67C), C111(H11J,H11K,H11L), C29(H29A,H29B,
 H29C), C141(H14D,H14E,H14F), C71(H71A,H71B,H71C), C55(H55A,H55B,H55C),
 C150(H15G,H15H,H15I), C12(H12J,H12K,H12L), C157(H15J,H15K,H15L), C106(H10G,
 H10H,H10I), C109(H10J,H10K,H10L), C158(H15M,H15N,H15O), C70(H70A,H70B,H70C),
 C110(H11M,H11N,H11O), C115(H11P,H11Q,H11R), C140(H14G,H14H,H14I), C155(H15P,
 H15Q,H15R), C113(H11S,H11T,H11U), C97(H97A,H97B,H97C), C54(H54A,H54B,H54C),
 C80(H80A,H80B,H80C), C31(H31A,H31B,H31C), C21(H21A,H21B,H21C), C68(H68A,H68B,
 H68C), C74(H74A,H74B,H74C), C75(H75A,H75B,H75C), C63(H63A,H63B,H63C), C76(H76A,
 H76B,H76C), C19(H19A,H19B,H19C), C72(H72A,H72B,H72C), C114(H11V,H11W,H11X),
 C20(H20A,H20B,H20C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C11(H11Y,H,HA),
 C165(H16A,H16B,H16C), C166(H16D,H16E,H16F), C167(H16G,H16H,H16I), C172(H17A,
 H17B,H17C), C173(H17D,H17E,H17F), C174(H17G,H17H,H17I), C161(H16J,H16K,H16L),
 C162(H16M,H16N,H16O), C169(H16P,H16Q,H16R), C163(H16S,H16T,H16U), C171(H17J,
 H17K,H17L), C170(H17M,H17N,H17O), C154(H15S,H15T,H15U), C153(H15V,H15W,H15X)
;