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_7044440
_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         'C66 H48 Mn4 N10 O14, 2(F6 P), 1.5(C4 O)'
_chemical_formula_sum            'C72 H48 F12 Mn4 N10 O15.5 P2'
_chemical_formula_weight         1810.90
_chemical_name_common            'Galia21 (Masha)'
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_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                90
_cell_angle_beta                 106.0360(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.4080(2)
_cell_length_b                   20.7610(3)
_cell_length_c                   26.8660(5)
_cell_measurement_reflns_used    13280
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.72
_cell_measurement_theta_min      0.79
_cell_volume                     7723.6(2)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.075
_diffrn_reflns_av_unetI/netI     0.0672
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            13159
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.719
_diffrn_reflns_theta_max         24.719
_diffrn_reflns_theta_min         1.259
_exptl_absorpt_coefficient_mu    0.781
_exptl_absorpt_correction_T_max  0.8522
_exptl_absorpt_correction_T_min  0.7835
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'  
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3648
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_exptl_transmission_factor_max   0.8522
_exptl_transmission_factor_min   0.7835
_refine_diff_density_max         1.812
_refine_diff_density_min         -0.598
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1033
_refine_ls_number_reflns         13159
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1254
_refine_ls_R_factor_gt           0.0720
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1446P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1939
_refine_ls_wR_factor_ref         0.2218
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7942
_reflns_number_total             13159
_reflns_threshold_expression     'I > 2\s(I)'
_cod_depositor_comments
;

2018-06-11
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C144 H96 F24 Mn8 N20 O31 P4'
_cod_original_formula_weight         3621.80
_cod_original_formula_moiety         '2(C66 H48 Mn4 N10 O14), 4(F6 P), 3(C4 O)'
_cod_original_formula_units_Z            2
_cod_data_source_file            c7dt03387g2.cif
_cod_data_source_block           galia21
_cod_database_code               7044440
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.872
_shelx_estimated_absorpt_t_min   0.800
_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. Restrained distances
 C72-C71
 1.5 with sigma of 0.001
 O16-C72
 1.4 with sigma of 0.001
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C15(H15), C16(H16), C18(H18),
 C19(H19), C20(H20), C26(H26), C27(H27), C29(H29), C30(H30), C31(H31), C37(H37),
  C38(H38), C40(H40), C41(H41), C42(H42), C48(H48), C49(H49), C51(H51),
 C52(H52), C53(H53), C59(H59), C60(H60), C62(H62), C63(H63), C64(H64)
3.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C12(H12A,H12B,H12C), C23(H23A,H23B,H23C), C34(H34A,H34B,
 H34C), C45(H45A,H45B,H45C), C56(H56A,H56B,H56C)
;
_olex2_submission_special_instructions 'No special instructions were received'