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_7043039
_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         'C44 H84 Ga2 P2 Si2'
_chemical_formula_sum            'C44 H84 Ga2 P2 Si2'
_chemical_formula_weight         870.67
_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             2016-11-24
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_audit_update_record
;
2017-02-23 deposited with the CCDC.
2017-05-01 downloaded from the CCDC.
;
_cell_angle_alpha                101.3830(10)
_cell_angle_beta                 104.321(2)
_cell_angle_gamma                96.903(2)
_cell_formula_units_Z            2
_cell_length_a                   11.8035(5)
_cell_length_b                   12.1037(5)
_cell_length_c                   18.2645(8)
_cell_measurement_reflns_used    9990
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      26.429
_cell_measurement_theta_min      2.328
_cell_volume                     2439.01(18)
_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      110.0
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 0.998
_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  0.0293
_diffrn_reflns_av_unetI/netI     0.0197
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            59532
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.447
_diffrn_reflns_theta_min         2.328
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.246
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6022
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1438 before and 0.0409 after correction.
The Ratio of minimum to maximum transmission is 0.8079.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.186
_exptl_crystal_description       block
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.489
_exptl_crystal_size_mid          0.229
_exptl_crystal_size_min          0.168
_refine_diff_density_max         0.310
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.044
_refine_ls_extinction_coef       0.0021(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         10027
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0214
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0190P)^2^+1.1140P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0476
_refine_ls_wR_factor_ref         0.0495
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8986
_reflns_number_total             10027
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00950j2.cif
_cod_data_source_block           compound1
_cod_database_code               7043039
_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.a Aromatic/amide H refined with riding coordinates:
 C30(H30), C26(H26), C44(H44), C40(H40), C29(H29), C27(H27), C28(H28),
 C41(H41), C42(H42), C43(H43)
2.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C14(H14A,H14B,H14C), C23(H23A,H23B,H23C), C16(H16A,H16B,
 H16C), C8(H8A,H8B,H8C), C24(H24A,H24B,H24C), C34(H34A,H34B,H34C), C32(H32A,
 H32B,H32C), C22(H22A,H22B,H22C), C15(H15A,H15B,H15C), C33(H33A,H33B,H33C),
 C4(H4A,H4B,H4C), C37(H37A,H37B,H37C), C3(H3A,H3B,H3C), C38(H38A,H38B,H38C),
 C11(H11A,H11B,H11C), C2(H2A,H2B,H2C), C12(H12A,H12B,H12C), C36(H36A,H36B,H36C),
  C6(H6A,H6B,H6C), C20(H20A,H20B,H20C), C10(H10A,H10B,H10C), C18(H18A,H18B,
 H18C), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              86910
_shelx_shelxl_version_number     2016/6
_olex2_submission_special_instructions 'No special instructions were received'