Synthesis of Trinuclear Tin(II), Germanium(II), and Aluminum(III) Cyclophane Complexes
Ermert, David M.; Gordon, Jesse B.; Abboud, Khalil A.; Murray, Leslie J.; Organometallics 35 (2016) 3651–; doi:10.1021/acs.organomet.6b00354

data_4088725
_publ_section_title
;
 Synthesis of Trinuclear Tin(II), Germanium(II), and Aluminum(III)
 Cyclophane Complexes
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              3651
_journal_paper_doi               10.1021/acs.organomet.6b00354
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C52 H84 N6 Al3, 2(C7 H8)'
_chemical_formula_sum            'C66 H100 Al3 N6'
_chemical_formula_weight         1058.46
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-04-17 # Formatted by publCIF

;
_cell_angle_alpha                90
_cell_angle_beta                 90.647(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.0700(5)
_cell_length_b                   14.1602(4)
_cell_length_c                   24.3189(7)
_cell_measurement_reflns_used    9456
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.0
_cell_volume                     6566.5(3)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2 (Bruker, 2008)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2008)'
_computing_molecular_graphics    'XP in SHELXTL-plus, Bruker 2014'
_computing_publication_material  'SHELXL2014/7, Sheldrick, G. M. 2014'
_computing_structure_refinement  'SHELXL2014/7, Sheldrick G. M. 2014'
_computing_structure_solution    'SHELXL2014/7, Sheldrick G. M. 2014'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker APEX-II DUO'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0667
_diffrn_reflns_av_unetI/netI     0.0462
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            56828
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        66.481
_diffrn_reflns_theta_max         66.481
_diffrn_reflns_theta_min         3.612
_diffrn_source                   'I\mS microsource'
_exptl_absorpt_coefficient_mu    0.834
_exptl_absorpt_correction_T_max  0.9749
_exptl_absorpt_correction_T_min  0.8895
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
'based on measured indexed crystal faces, Bruker SHELXTL2014 (Sheldrick, 2014)'
_exptl_crystal_colour            colourless
_exptl_crystal_description       plates
_exptl_crystal_F_000             2308
_exptl_crystal_size_max          0.189
_exptl_crystal_size_mid          0.141
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.889
_refine_diff_density_min         -0.650
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     553
_refine_ls_number_reflns         11275
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0840
_refine_ls_R_factor_gt           0.0745
_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^)+(0.0646P)^2^+15.5245P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1889
_refine_ls_wR_factor_ref         0.1932
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9436
_reflns_number_total             11275
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00354_si_002.cif
_cod_data_source_block           murr6
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4088725
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              10407
_shelx_hkl_checksum              86234
_shelx_fab_checksum              43796