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_7021696
_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_formula_moiety         'C58 H48 Cu2 N8, 2(C18 H12 O6 As)'
_chemical_formula_sum            'C94 H72 As2 Cu2 N8 O12'
_chemical_formula_weight         1782.52
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.195(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.5080(5)
_cell_length_b                   17.4618(5)
_cell_length_c                   28.2773(9)
_cell_measurement_reflns_used    8467
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      20.01
_cell_measurement_theta_min      2.43
_cell_volume                     8151.2(4)
_computing_cell_refinement       'Bruker SAINT v7.56A'
_computing_data_collection       'Bruker APEX-II v2009-1'
_computing_data_reduction        'Bruker SAINT v7.56A'
_computing_molecular_graphics    'XP (Sheldrick, 2008)'
_computing_publication_material  'CIFTab (Sheldrick, 2012)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 0.997
_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  'channel-cut Si-<111> crystal'
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77490
_diffrn_reflns_av_R_equivalents  0.0936
_diffrn_reflns_av_unetI/netI     0.1416
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            98832
_diffrn_reflns_theta_full        27.24
_diffrn_reflns_theta_max         27.24
_diffrn_reflns_theta_min         0.79
_exptl_absorpt_coefficient_mu    1.698
_exptl_absorpt_correction_T_max  0.9352
_exptl_absorpt_correction_T_min  0.8485
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Sheldrick, 2008'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blade
_exptl_crystal_F_000             3648
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         3.098
_refine_diff_density_min         -0.738
_refine_diff_density_rms         0.148
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.018(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2126
_refine_ls_number_reflns         27567
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.1722
_refine_ls_R_factor_gt           0.0865
_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^)+(0.1662P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2182
_refine_ls_wR_factor_ref         0.2786
_reflns_number_gt                14011
_reflns_number_total             27567
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt50971k.txt
_cod_data_source_block           nd019a
_cod_original_cell_volume        8151.1(4)
_cod_original_sg_symbol_H-M      'P 2(1)'
_cod_database_code               7021696