Synthesis and structural characterization of iron complexes bearing N-aryl-phenanthren-o-iminoquinone ligands.
Xu, Bin; Ma, Anjie; Jia, Teng; Hao, Zhiqiang; Gao, Wei; Mu, Ying; Dalton transactions (Cambridge, England : 2003) 45 (2016) 17966–17973; doi:10.1039/c6dt03572h

data_7040873
_publ_section_title
;
 Synthesis and structural characterization of iron complexes bearing
 N-aryl-phenanthren-o-iminoquinone ligands.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17966
_journal_page_last               17973
_journal_paper_doi               10.1039/c6dt03572h
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         '2(C44 H34 Cl Fe N2 O2), C7 H8, 2(Cl4 Fe)'
_chemical_formula_sum            'C95 H76 Cl10 Fe4 N4 O4'
_chemical_formula_weight         1915.49
_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   geom
_audit_creation_date             2016-03-17
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-03-18 deposited with the CCDC.
2016-10-11 downloaded from the CCDC.
;
_cell_angle_alpha                63.6670(10)
_cell_angle_beta                 66.6300(10)
_cell_angle_gamma                68.4790(10)
_cell_formula_units_Z            1
_cell_length_a                   13.3556(8)
_cell_length_b                   14.2676(8)
_cell_length_c                   14.3243(8)
_cell_measurement_reflns_used    3307
_cell_measurement_temperature    184.65
_cell_measurement_theta_max      25.91
_cell_measurement_theta_min      2.63
_cell_volume                     2184.3(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      184.65
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0186
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11789
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.028
_diffrn_reflns_theta_min         1.637
_exptl_absorpt_coefficient_mu    1.011
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_description       block
_exptl_crystal_F_000             980
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.585
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     552
_refine_ls_number_reflns         8425
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0488
_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^)+(0.0611P)^2^+0.6637P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1101
_refine_ls_wR_factor_ref         0.1227
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6196
_reflns_number_total             8425
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt03572h2.cif
_cod_data_source_block           complex_3a
_cod_depositor_comments
'Adding full bibliography for 7040871--7040875.cif.'
_cod_database_code               7040873
_shelx_estimated_absorpt_t_max   0.847
_shelx_estimated_absorpt_t_min   0.808
_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. Rigid bond restraints
 C53, C54, C55, C56, C57, C58, C59
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Others
 Fixed Sof: C53(0.5) H53(0.5) C54(0.5) H54(0.5) C55(0.5) H55(0.5) C56(0.5)
 C57(0.5) H57(0.5) C58(0.5) H58(0.5) C59(0.5) H59A(0.5) H59B(0.5) H59C(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C17(H17), C18(H18), C19(H19), C33(H33), C34(H34), C35(H35), C36(H36), C39(H39),
  C40(H40), C41(H41), C42(H42), C47(H47), C48(H48), C49(H49), C53(H53),
 C54(H54), C55(H55), C57(H57), C58(H58)
4.b Fitted hexagon refined as free rotating group:
 C53(C54,C55,C56,C57,C58)
4.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C51(H51A,H51B,H51C), C52(H52A,H52B,
 H52C), C59(H59A,H59B,H59C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'