Design, synthesis and crystal structure of a copper dimetallocyclophane complex exhibiting unique rotational isomerism
McNelis, Brian J.; Nathan, Lawrence C.; Clark, Curtis J.; Journal of the Chemical Society, Dalton Transactions  (1999) 1831–; doi:10.1039/a807579d

data_7027130
_publ_contact_author
;       Brian J. McNelis
        Department of Chemistry
        Santa Clara University
        500 El Camino Real
        Santa Clara, CA  95053-0270
        U.S.A.
;
_publ_section_title
;
 Design, synthesis and crystal structure of a copper dimetallocyclophane
 complex exhibiting unique rotational isomerism
;
_journal_issue                   11
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1831
_journal_paper_doi               10.1039/a807579d
_journal_year                    1999
_chemical_formula_sum            'C45 H39 Cu2 N5 O6'
_chemical_formula_weight         872.89
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   'difmap; geom for nitromethane'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 115.257(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   29.647(3)
_cell_length_b                   14.834(3)
_cell_length_c                   19.991(2)
_cell_measurement_reflns_used    35
_cell_measurement_temperature    183
_cell_measurement_theta_max      13.50
_cell_measurement_theta_min      4.61
_cell_volume                     7951(2)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_sigmaI/netI    0.0669
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            8086
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.11
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.126
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6780
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_description       block
_exptl_crystal_F_000             3600
_exptl_crystal_size_max          .46
_exptl_crystal_size_mid          .38
_exptl_crystal_size_min          .26
_refine_diff_density_max         0.548
_refine_diff_density_min         -0.643
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.020
_refine_ls_goodness_of_fit_obs   1.067
_refine_ls_hydrogen_treatment    'ref all except nitromethane methyl'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     668
_refine_ls_number_reflns         7009
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_restrained_S_obs      1.067
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_obs          0.0453
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0569P)^2^+1.4674P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1208
_refine_ls_wR_factor_obs         0.1069
_reflns_number_observed          5238
_reflns_number_total             7010
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            807579dsup1.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0569P)^2^+1.4674P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0569P)^2^+1.4674P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        7951.3(19)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7027130