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_4088726
_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         'C45 H63 N6 Cl3 Ge3, 3.5(C6 H6)'
_chemical_formula_sum            'C66 H84 Cl3 Ge3 N6'
_chemical_formula_weight         1285.51
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_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                 100.8793(12)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   44.808(3)
_cell_length_b                   18.1308(13)
_cell_length_c                   15.9563(11)
_cell_measurement_reflns_used    9723
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.0
_cell_volume                     12730.0(15)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II DUO'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       58
_diffrn_reflns_limit_h_min       -57
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            120311
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         0.925
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.578
_exptl_absorpt_correction_T_max  0.9062
_exptl_absorpt_correction_T_min  0.7933
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
'based on measured indexed crystal faces, Bruker SHELXTL2014 (Sheldrick, 2014)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_description       Blocks
_exptl_crystal_F_000             5352
_exptl_crystal_size_max          0.235
_exptl_crystal_size_mid          0.183
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.828
_refine_diff_density_min         -0.879
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     682
_refine_ls_number_reflns         14650
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0304
_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^)+(0.0460P)^2^+16.5724P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0815
_refine_ls_wR_factor_ref         0.0853
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12268
_reflns_number_total             14650
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00354_si_002.cif
_cod_data_source_block           murr14
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4088726
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.708
_shelx_estimated_absorpt_t_max   0.898
_shelx_res_checksum              54829
_shelx_hkl_checksum              350