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_7021699
_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         'C87 H72 Cu3 N12, 3(C18 H12 As O6), 3(H2 O)'
_chemical_formula_sum            'C141 H114 As3 Cu3 N12 O21'
_chemical_formula_weight         2727.81
_chemical_name_systematic
;
 ?
;
_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                 98.473(2)
_cell_angle_gamma                90
_cell_formula_units_Z            6
_cell_length_a                   20.9348(6)
_cell_length_b                   17.0379(5)
_cell_length_c                   58.1561(17)
_cell_measurement_reflns_used    9921
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      17.02
_cell_measurement_theta_min      1.30
_cell_volume                     20517.0(10)
_computing_cell_refinement       'Bruker SAINT v7.68A'
_computing_data_collection       'Bruker APEX-II v2010-7'
_computing_data_reduction        'Bruker SAINT v7.68A'
_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      120(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.585
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker Kappa X8-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  0.1126
_diffrn_reflns_av_unetI/netI     0.1569
_diffrn_reflns_Laue_measured_fraction_full 0.585
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            137432
_diffrn_reflns_point_group_measured_fraction_full 0.578
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         20.926
_diffrn_reflns_theta_min         0.983
_exptl_absorpt_coefficient_mu    1.252
_exptl_absorpt_correction_T_max  0.7446
_exptl_absorpt_correction_T_min  0.5909
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick, 2008'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_description       rod
_exptl_crystal_F_000             8388
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.278
_refine_diff_density_min         -0.895
_refine_diff_density_rms         0.149
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.14(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1496
_refine_ls_number_reflns         42913
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1589
_refine_ls_R_factor_gt           0.1193
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1381P)^2^+257.6131P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2793
_refine_ls_wR_factor_ref         0.3022
_reflns_Friedel_coverage         0.907
_reflns_Friedel_fraction_full    0.570
_reflns_Friedel_fraction_max     0.979
_reflns_number_gt                28437
_reflns_number_total             42913
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3dt50971k.txt
_cod_data_source_block           nd1024
_cod_database_code               7021699
_shelxl_version_number           2012-9