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_7044441
_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         'C26 H20 Co N5 O2, F6 P, C4 H10 O'
_chemical_formula_sum            'C30 H30 Co F6 N5 O3 P'
_chemical_formula_weight         712.49
_chemical_name_common            'Galia8 (Masha)'
_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                78.154(3)
_cell_angle_beta                 76.135(4)
_cell_angle_gamma                83.078(4)
_cell_formula_units_Z            2
_cell_length_a                   8.4690(3)
_cell_length_b                   12.5680(8)
_cell_length_c                   15.2380(10)
_cell_measurement_reflns_used    4448
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.14
_cell_measurement_theta_min      2.36
_cell_volume                     1536.77(15)
_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 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0336
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4513
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.360
_exptl_absorpt_coefficient_mu    0.688
_exptl_absorpt_correction_T_max  0.9120
_exptl_absorpt_correction_T_min  0.8401
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'  
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             730
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   0.902
_exptl_transmission_factor_min   0.820
_refine_diff_density_max         0.551
_refine_diff_density_min         -0.505
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         4513
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0385
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0528P)^2^+1.2026P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.1014
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3968
_reflns_number_total             4513
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03387g2.cif
_cod_data_source_block           galia8
_cod_database_code               7044441
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.922
_shelx_estimated_absorpt_t_min   0.820
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Riding coordinates:
 C15(H15)
2.b Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C29(H29A,H29B)
2.c Me refined with riding coordinates:
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C30(H30A,H30B,H30C)
2.d Aromatic/amide H refined with riding coordinates:
 N5(H5), C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C12(H12),
 C13(H13), C14(H14), C17(H17), C18(H18), C19(H19), C22(H22), C23(H23)
;
_olex2_submission_special_instructions 'No special instructions were received'