Box-like Heterometallic Macrocycles Derived from Bis-Terpyridine Metalloligands
Liu, Jing-Jing; Lin, Yue-Jian; Jin, Guo-Xin; Organometallics 33 (2014) 1283–; doi:10.1021/om500093p

data_4082786
_publ_section_title
;
 Box-like Heterometallic Macrocycles Derived from Bis-Terpyridine
 Metalloligands
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1283
_journal_paper_doi               10.1021/om500093p
_journal_volume                  33
_journal_year                    2014
_chemical_formula_sum            'C180 H178 Cu2 F36 N18 O24 P4 Rh4 S4'
_chemical_formula_weight         4452.23
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 104.0760(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.1031(4)
_cell_length_b                   29.3824(7)
_cell_length_c                   20.8407(5)
_cell_measurement_reflns_used    9892
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      68.23
_cell_measurement_theta_min      2.65
_cell_volume                     9564.7(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.935
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0609
_diffrn_reflns_av_unetI/netI     0.0672
_diffrn_reflns_Laue_measured_fraction_full 0.935
_diffrn_reflns_Laue_measured_fraction_max 0.932
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            46244
_diffrn_reflns_point_group_measured_fraction_full 0.935
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.998
_diffrn_reflns_theta_min         2.653
_exptl_absorpt_coefficient_mu    4.604
_exptl_absorpt_correction_T_max  0.753
_exptl_absorpt_correction_T_min  0.309
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_description       rod
_exptl_crystal_F_000             4524
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.080
_platon_squeeze_details
; 
 In asymmetric unit of this data, there were disordered 
 solvent molecules (one acetonitrile and one diethyl ether 
 molecules) which could not be restrained properly. 
 Therefore, SQUEEZE algorithm was used to omit them. 
;
_refine_diff_density_max         3.275
_refine_diff_density_min         -0.634
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1165
_refine_ls_number_reflns         16243
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.1143
_refine_ls_R_factor_gt           0.0905
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.1683P)^2^+21.5451P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2472
_refine_ls_wR_factor_ref         0.2690
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11710
_reflns_number_total             16243
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500093p_si_002.cif
_cod_data_source_block           3b
_cod_database_code               4082786
_shelx_estimated_absorpt_t_min   0.320
_shelx_estimated_absorpt_t_max   0.710
_shelxl_version_number           2013-2
_shelx_res_checksum              51491
_shelx_hkl_checksum              49704