Unfolding of the [Cu2(1,3-bis(9-methyl-1,10-phenanthrolin-2-yl)propane)2]2+ Helicate. Coupling of the Chlorocarbon Dehalogenation to the Unfolding Process
L. Lemus; J. Guerrero; J. Costamagna; G. Estiu; G. Ferraudi; A. Graham Lappin; A. Oliver; B. C. Noll; Inorganic Chemistry 49 (2010) 4023–4035; doi:10.1021/ic9018986

data_4315439
_publ_section_title
;
 Unfolding of the
 [Cu2(1,3-bis(9-methyl-1,10-phenanthrolin-2-yl)propane)2]2+ Helicate.
 Coupling of the Chlorocarbon Dehalogenation to the Unfolding Process
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4023
_journal_page_last               4035
_journal_paper_doi               10.1021/ic9018986
_journal_volume                  49
_journal_year                    2010
_chemical_compound_source        synthesized
_chemical_formula_moiety         'C58 H48 Cu2 N8, 2(Cl O4), C2 H3 N'
_chemical_formula_sum            'C60 H51 Cl2 Cu2 N9 O8'
_chemical_formula_weight         1224.08
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.9255(4)
_cell_length_b                   25.2671(5)
_cell_length_c                   25.3322(6)
_cell_measurement_reflns_used    9824
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.4479
_cell_measurement_theta_min      2.5381
_cell_volume                     10833.5(4)
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2004; Sheldrick, 2003)'
_computing_molecular_graphics    'XP (Sheldrick, 1998)'
_computing_publication_material  'XCIF (Sheldrick, 2001)/enCIFer (CCDC, 2004)'
_computing_structure_refinement  'XL (Sheldrick, 2001)'
_computing_structure_solution    'XS (Sheldrick, 2001)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker d8-Apex II CCD diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0710
_diffrn_reflns_av_sigmaI/netI    0.0300
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            191317
_diffrn_reflns_theta_full        26.41
_diffrn_reflns_theta_max         26.41
_diffrn_reflns_theta_min         1.61
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Siemens KFFMO2K-90'
_exptl_absorpt_coefficient_mu    0.951
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Sheldrick, G. M. (2007). SADABS. University of G\"ottingen, Germany.'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             5040
_exptl_crystal_size_max          0.216
_exptl_crystal_size_mid          0.093
_exptl_crystal_size_min          0.082
_refine_diff_density_max         1.016
_refine_diff_density_min         -0.614
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     735
_refine_ls_number_reflns         11107
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0385
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0446P)^2^+15.4220P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0921
_refine_ls_wR_factor_ref         0.1015
_reflns_number_gt                8654
_reflns_number_total             11107
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9018986_si_002_1.cif
_cod_data_source_block           bcn353_0m
_cod_database_code               4315439