Synthesis of a Rotaxane CuI Triazolide under Aqueous Conditions
Joby Winn; Aleksandra Pinczewska; Stephen M. Goldup; Journal of the American Chemical Society 135 (2013) 13318–13321; doi:10.1021/ja407446c

data_4120779
_publ_section_title
;
 Synthesis of a Rotaxane CuI Triazolide under Aqueous Conditions
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13318
_journal_page_last               13321
_journal_paper_doi               10.1021/ja407446c
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C62 H76 Cu N5 O2'
_chemical_formula_sum            'C62 H76 Cu N5 O2'
_chemical_formula_weight         986.81
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.0012(11)
_cell_length_b                   24.6026(13)
_cell_length_c                   25.8588(13)
_cell_measurement_reflns_used    9804
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      64.9936
_cell_measurement_theta_min      4.5100
_cell_volume                     12088.4(11)
_computing_cell_refinement       'SAINT V8.27B (Bruker AXS Inc., 2012)'
_computing_data_collection       'Bruker Instrument Service v2012.12.0.3'
_computing_data_reduction        'SAINT V8.27B (Bruker AXS Inc., 2012)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0669
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            92997
_diffrn_reflns_theta_full        66.72
_diffrn_reflns_theta_max         66.72
_diffrn_reflns_theta_min         3.40
_exptl_absorpt_coefficient_mu    0.832
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.73
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.084
_exptl_crystal_description       ' Block'
_exptl_crystal_F_000             4224
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.402
_refine_diff_density_min         -2.915
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     608
_refine_ls_number_reflns         10228
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.2245
_refine_ls_R_factor_gt           0.2194
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[\s^2^(Fo^2^)+(0.0304P)^2^+468.1467P]
where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4507
_refine_ls_wR_factor_ref         0.4524
_reflns_number_gt                9431
_reflns_number_total             10228
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja407446c_si_003.cif
_cod_data_source_block           I
_cod_database_code               4120779