Novel iminopyridine derivatives: ligands for preparation of Fe(ii) and Cu(ii) dinuclear complexes.
Martínez-Ferraté, Oriol; López-Valbuena, Josep M; Belmonte, Marta Martínez; White, Andrew J. P.; Benet-Buchholz, Jordi; Britovsek, George J. P.; Claver, Carmen; van Leeuwen, Piet W. N. M.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 3564–3576; doi:10.1039/c5dt04358a

data_7038030
_publ_section_title
;
 Novel iminopyridine derivatives: ligands for preparation of Fe(ii) and
 Cu(ii) dinuclear complexes.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3564
_journal_page_last               3576
_journal_paper_doi               10.1039/c5dt04358a
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety
'C80.83 H65.33 F6 Fe2 N10 O10.83 S2, 2(C F3 O3 S), (C2 H3 N)'
_chemical_formula_sum            'C84.83 H68.33 F12 Fe2 N11 O16.83 S4'
_chemical_formula_weight         1979.11
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-11-16 deposited with the CCDC.
2016-01-08 downloaded from the CCDC.
;
_cell_angle_alpha                114.155(2)
_cell_angle_beta                 98.1770(18)
_cell_angle_gamma                104.8208(19)
_cell_formula_units_Z            3
_cell_length_a                   13.0865(3)
_cell_length_b                   24.7981(6)
_cell_length_c                   24.8927(6)
_cell_measurement_reflns_used    18616
_cell_measurement_temperature    173
_cell_measurement_theta_max      29.5771
_cell_measurement_theta_min      2.9858
_cell_volume                     6840.8(3)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 15.9825
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.822
_diffrn_measurement_device_type  'OD Xcalibur 3'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_sigmaI/netI    0.0533
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            59011
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         29.64
_diffrn_reflns_theta_min         2.99
_exptl_absorpt_coefficient_mu    0.505
_exptl_absorpt_correction_T_max  0.937
_exptl_absorpt_correction_T_min  0.879
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) 
(compiled Aug  3 2011,13:03:54) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
;
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             3039
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.17
_platon_squeeze_details
;
 SQUEEZE suggested 69 e/cell = 34.5 e/asu = 23 e/Fe2 complex
 The coordinated solvents are MeCN (C2H3N = 22e) and dmf (C3H7NO = 40e)
 The solvent before SQUEEZE looked most like MeCN
 1MeCN = (1 x 22) = 22e so this was used as the solvent present.
 
 Thus Fe2 complex is low by 1(C2H3N) = C2 H3 N, and the UNIT low by
 C6 H9 N3, i.e. C248.5 H196 N30 O50.5 F36 S12 Fe6
;
_refine_diff_density_max         1.255
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1909
_refine_ls_number_reflns         31759
_refine_ls_number_restraints     703
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.1010
_refine_ls_R_factor_gt           0.0721
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1302P)^2^+2.1591P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2104
_refine_ls_wR_factor_ref         0.2318
_reflns_number_gt                22109
_reflns_number_total             31759
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt04358a2.cif
_cod_data_source_block           16
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7038024--7038030.cif.
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7038030