Resolution and characterization of helicate dimer and trimer complexes of 1,3-bis(9-methyl-1,10-phenanthrolin-2-yl)propane with copper(i).
Lemus, Luis; Guerrero, Juan; Costamagna, Juan; Lorca, Romina; Jara, Danilo H.; Ferraudi, Guillermo; Oliver, Allen; Lappin, A. Graham; Dalton transactions (Cambridge, England : 2003) 42 (2013) 11426–11435; doi:10.1039/c3dt50971k

data_7021697
_publ_section_title
;
 Resolution and characterization of helicate dimer and trimer complexes of
 1,3-bis(9-methyl-1,10-phenanthrolin-2-yl)propane with copper(i).
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11426
_journal_page_last               11435
_journal_paper_doi               10.1039/c3dt50971k
_journal_volume                  42
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C58 H48 Cu2 N8 , 2(C18 H12 O6 As) 2(C2 H3 N)'
_chemical_formula_sum            'C98 H78 As2 Cu2 N10 O12'
_chemical_formula_weight         1864.62
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 90.228(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.1177(6)
_cell_length_b                   17.4161(6)
_cell_length_c                   28.7700(9)
_cell_measurement_reflns_used    5013
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.37
_cell_measurement_theta_min      2.26
_cell_volume                     8576.9(5)
_computing_cell_refinement       'Bruker SAINT v7.66A'
_computing_data_collection       'Bruker APEX-II v2009-9'
_computing_data_reduction        'Bruker SAINT v7.66A'
_computing_molecular_graphics    'XP (Sheldrick, 2008)'
_computing_publication_material  'CIFTab (Sheldrick, 2012)'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.803
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       'combination of \w and \f-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  0.0736
_diffrn_reflns_av_unetI/netI     0.1059
_diffrn_reflns_Laue_measured_fraction_full 0.803
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            86434
_diffrn_reflns_point_group_measured_fraction_full 0.778
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         23.358
_diffrn_reflns_theta_min         0.708
_exptl_absorpt_coefficient_mu    1.332
_exptl_absorpt_correction_T_max  0.8929
_exptl_absorpt_correction_T_min  0.7027
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS, Sheldrick, 2008'
_exptl_crystal_colour            orange/red
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_description       blade
_exptl_crystal_F_000             3824
_exptl_crystal_size_max          0.285
_exptl_crystal_size_mid          0.097
_exptl_crystal_size_min          0.087
_refine_diff_density_max         1.374
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.128
_refine_ls_abs_structure_details
;
 Flack x determined using 5515 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.037(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2185
_refine_ls_number_reflns         24173
_refine_ls_number_restraints     1509
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.1267
_refine_ls_R_factor_gt           0.0791
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1267P)^2^+25.5625P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2007
_refine_ls_wR_factor_ref         0.2312
_reflns_Friedel_coverage         0.871
_reflns_Friedel_fraction_full    0.752
_reflns_Friedel_fraction_max     0.938
_reflns_number_gt                16237
_reflns_number_total             24173
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3dt50971k.txt
_cod_data_source_block           nd1014z
_cod_database_code               7021697
_shelx_estimated_absorpt_t_min   0.703
_shelx_estimated_absorpt_t_max   0.893
_shelxl_version_number           2012-9