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_4088727
_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 Sn3, 4(C4H8O1)'
_chemical_formula_sum            'C61 H95 Cl3 N6 O4 Sn3'
_chemical_formula_weight         1438.84
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2013-12-17 # Formatted by publCIF

;
_cell_angle_alpha                85.9477(17)
_cell_angle_beta                 82.3548(16)
_cell_angle_gamma                76.8208(16)
_cell_formula_units_Z            4
_cell_length_a                   16.0779(16)
_cell_length_b                   18.9798(19)
_cell_length_c                   22.291(2)
_cell_measurement_reflns_used    9810
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.0
_cell_volume                     6558.4(11)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2 (Bruker, 2008)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2008)'
_computing_molecular_graphics    'SHELXL-2013 (Sheldrick, 2013)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.969
_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  0.0793
_diffrn_reflns_av_unetI/netI     0.1249
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            52355
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         0.922
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.304
_exptl_absorpt_correction_T_max  0.8491
_exptl_absorpt_correction_T_min  0.7339
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
'based on measured indexed crystal faces, Bruker SHELXTL  v6.14 (Bruker 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_description       Irregular
_exptl_crystal_F_000             2944
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.681
_refine_diff_density_min         -1.487
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.877
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1051
_refine_ls_number_reflns         29170
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.877
_refine_ls_R_factor_all          0.0824
_refine_ls_R_factor_gt           0.0477
_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^)+(0.0366P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1065
_refine_ls_wR_factor_ref         0.1159
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17287
_reflns_number_total             29170
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00354_si_002.cif
_cod_data_source_block           jess16
_cod_database_code               4088727
_shelxl_version_number           2013-3
_shelx_res_checksum              42835
_shelx_hkl_checksum              87832