Heteroleptic Complexes via Solubility Control: Examples of Cu(II), Co(II), Ni(II) and Mn(II) complexes Based on the Derivatives of Terpyridine and Hydroxyquinoline
Baskin, Maria; Fridman, Natalia; Kosa, Monica; Maayan, Galia; Dalton Trans.  (2017) –; doi:10.1039/C7DT03387G

data_7044438
_publ_section_title
;
 Heteroleptic Complexes via Solubility Control: Examples of Cu(II),
 Co(II), Ni(II) and Mn(II) complexes Based on the Derivatives of
 Terpyridine and Hydroxyquinoline
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT03387G
_journal_year                    2017
_chemical_formula_moiety
'C43 H34 Cu2 N9 O2, 0.5(C8), 3(F6 P), 2(C2 H3 N), C2 N'
_chemical_formula_sum            'C53 H40 Cu2 F18 N12 O2 P3'
_chemical_formula_weight         1438.96
_chemical_name_common            'Galia23 (Masha)'
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-09-28
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-09-28 deposited with the CCDC.
2017-10-09 downloaded from the CCDC.
;
_cell_angle_alpha                91.421(7)
_cell_angle_beta                 97.104(5)
_cell_angle_gamma                104.077(6)
_cell_formula_units_Z            2
_cell_length_a                   10.3030(11)
_cell_length_b                   12.5250(18)
_cell_length_c                   24.583(4)
_cell_measurement_reflns_used    10011
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      0.905
_cell_measurement_theta_min      0.729
_cell_volume                     3048.5(7)
_computing_cell_refinement       'DENZO HKL2000 (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius, 2006)'
_computing_data_reduction        'DENZO HKL2000 (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200.15
_diffrn_detector_area_resol_mean 95
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'phi- and omega-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.088
_diffrn_reflns_av_unetI/netI     0.0765
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            10011
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.430
_diffrn_reflns_theta_max         24.430
_diffrn_reflns_theta_min         0.836
_exptl_absorpt_coefficient_mu    0.883
_exptl_absorpt_correction_T_max  24.430
_exptl_absorpt_correction_T_min  0.836
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'  
;
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1446
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_exptl_transmission_factor_max   0.883
_exptl_transmission_factor_min   0.759
_refine_diff_density_max         1.677
_refine_diff_density_min         -0.678
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     784
_refine_ls_number_reflns         10011
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1419
_refine_ls_R_factor_gt           0.0888
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1425P)^2^+6.8043P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2233
_refine_ls_wR_factor_ref         0.2554
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6440
_reflns_number_total             10011
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03387g2.cif
_cod_data_source_block           galia23
_cod_original_cell_volume        3048.5(8)
_cod_database_code               7044438
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.925
_shelx_estimated_absorpt_t_min   0.759
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8A), C9(H9), C12(H12), C13(H13),
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C22(H22), C23(H23),
  C24(H24), C27(H27), C28(H28), C29(H29), C30(H30), C32(H32), C33(H33),
 C34(H34), C36(H36), C37(H37)
2.b Idealised Me refined as rotating group:
 C41(H41A,H41B,H41C), C123(H12A,H12B,H12C), C43(H43A,H43B,H43C), C45(H45A,H45B,
 H45C)
;
_olex2_submission_special_instructions 'No special instructions were received'