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_7044439
_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         'C19 H17 Mn N3 O4, H2 O'
_chemical_formula_sum            'C19 H19 Mn N3 O5'
_chemical_formula_weight         424.31
_chemical_name_common            'Galia25 (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                83.00(3)
_cell_angle_beta                 83.70(5)
_cell_angle_gamma                83.759(14)
_cell_formula_units_Z            2
_cell_length_a                   8.420(3)
_cell_length_b                   10.766(3)
_cell_length_c                   10.903(2)
_cell_measurement_reflns_used    3006
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.70
_cell_measurement_theta_min      1.91
_cell_volume                     970.5(5)
_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 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.070
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3188
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        24.480
_diffrn_reflns_theta_max         24.480
_diffrn_reflns_theta_min         1.891
_exptl_absorpt_coefficient_mu    0.715
_exptl_absorpt_correction_T_max  0.9284
_exptl_absorpt_correction_T_min  0.8303
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'  
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             438
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.09
_exptl_transmission_factor_max   0.928
_exptl_transmission_factor_min   0.830
_refine_diff_density_max         0.314
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.289
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         3188
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.289
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0506
_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^)+(0.0441P)^2^+0.8187P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1168
_refine_ls_wR_factor_ref         0.1194
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2941
_reflns_number_total             3188
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03387g2.cif
_cod_data_source_block           galia25
_cod_database_code               7044439
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.938
_shelx_estimated_absorpt_t_min   0.830
_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(H8), C9(H9), C12(H12), C13(H13),
 C14(H14), C15(H15)
2.b Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C19(H19A,H19B,H19C)
;
_olex2_submission_special_instructions 'No special instructions were received'