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_7021698
_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         'C87 H72 Cu3 N12 , 3(Cl O4)'
_chemical_formula_sum            'C87 H72 Cl3 Cu3 N12 O12'
_chemical_formula_weight         1774.54
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           163
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3 2c'
_symmetry_space_group_name_H-M   'P -3 1 c'
_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                120.00
_cell_formula_units_Z            2
_cell_length_a                   16.9700(5)
_cell_length_b                   16.9700(5)
_cell_length_c                   17.6573(6)
_cell_measurement_reflns_used    9874
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.42
_cell_measurement_theta_min      2.52
_cell_volume                     4403.7(2)
_computing_cell_refinement       'Bruker SAINT v7.60A'
_computing_data_collection       'Bruker APEX-II v2009-7'
_computing_data_reduction        'Bruker SAINT v7.60A'
_computing_molecular_graphics
;
XP (Sheldrick, 2008) / Diamond 3.2i ((Brandenburg, 2012) / 
POV-ray v3.6.2 (Cason, 2003)
;
_computing_publication_material  'CIFTab (Sheldrick, 2012)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0655
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            64420
_diffrn_reflns_theta_full        29.01
_diffrn_reflns_theta_max         29.01
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    1.102
_exptl_absorpt_correction_T_max  0.9368
_exptl_absorpt_correction_T_min  0.9268
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick, 2008'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.237
_refine_diff_density_min         -0.569
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3028
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0716
_refine_ls_R_factor_gt           0.0646
_refine_ls_shift/su_max          0.092
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1659P)^2^+4.2969P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2195
_refine_ls_wR_factor_ref         0.2302
_reflns_number_gt                2623
_reflns_number_total             3028
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt50971k.txt
_cod_data_source_block           nd029a
_cod_original_sg_symbol_H-M      P-31c
_cod_database_code               7021698