Solvatomorphism and anion effects in predominantly low spin iron(iii) Schiff base complexes.
Boonprab, Theerapoom; Harding, Phimphaka; Murray, Keith S.; Phonsri, Wasinee; Telfer, Shane G.; Alkaş, Adil; Ketkaew, Rangsiman; Tantirungrotechai, Yuthana; Jameson, Guy N. L.; Harding, David J.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 12449–12458; doi:10.1039/c8dt02016g

data_7047318
_publ_section_title
;
 Solvatomorphism and anion effects in predominantly low spin iron(iii)
 Schiff base complexes.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12449
_journal_page_last               12458
_journal_paper_doi               10.1039/c8dt02016g
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'I, C30 H34 Fe N4 O2'
_chemical_formula_sum            'C30 H34 Fe I N4 O2'
_chemical_formula_weight         665.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-05-10
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5375)
;
_audit_update_record
;
2018-08-17 deposited with the CCDC.
2018-08-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.591(8)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.203(3)
_cell_length_b                   21.769(3)
_cell_length_c                   19.850(4)
_cell_measurement_reflns_used    1000
_cell_measurement_temperature    293
_cell_measurement_theta_max      70
_cell_measurement_theta_min      7
_cell_volume                     6636(2)
_computing_cell_refinement       'FSProcess in Process-Auto (Rigaku, 1998)'
_computing_data_collection       'CrystalClear (Rigaku, 2005)'
_computing_data_reduction        'FSProcess in Process-Auto (Rigaku, 1998)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'Image Plate'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_type            'Rigaku IP'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
scan:
    Number of images: 74
               Slice: 20.0000 - 205.0000
         Image width: 2.5000
            Exp time: 60.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 270.0000
                 XTD: 127.4000
              2theta: 0.0000
scan:
    Number of images: 72
               Slice: 24.0000 - 204.0000
         Image width: 2.5000
            Exp time: 60.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 0.0000
                 XTD: 127.4000
              2theta: 0.0000
scan:
    Number of images: 56
               Slice: 20.0000 - 160.0000
         Image width: 2.5000
            Exp time: 60.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 180.0000
                 XTD: 127.4000
              2theta: 0.0000
scan:
    Number of images: 44
               Slice: 75.0000 - 185.0000
         Image width: 2.5000
            Exp time: 60.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 90.0000
                 XTD: 127.4000
              2theta: 0.0000
;
_diffrn_measurement_device       'Crystal Goniometer'
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IP'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       FS_PROCESS
_diffrn_orient_matrix_UB_11      0.026807
_diffrn_orient_matrix_UB_12      0.039316
_diffrn_orient_matrix_UB_13      0.023408
_diffrn_orient_matrix_UB_21      0.045399
_diffrn_orient_matrix_UB_22      -0.023610
_diffrn_orient_matrix_UB_23      0.032548
_diffrn_orient_matrix_UB_31      0.006728
_diffrn_orient_matrix_UB_32      0.002664
_diffrn_orient_matrix_UB_33      -0.057017
_diffrn_radiation_monochromator  'Osmic Optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.2705
_diffrn_reflns_av_unetI/netI     0.1888
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9706
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        30.922
_diffrn_reflns_theta_max         30.922
_diffrn_reflns_theta_min         5.762
_diffrn_source                   'Rigaku MM007 rotating anode'
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.178
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.148
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2696
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.746
_refine_diff_density_min         -0.474
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.220
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         1018
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.177
_refine_ls_R_factor_all          0.1024
_refine_ls_R_factor_gt           0.1005
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2551
_refine_ls_wR_factor_ref         0.2618
_reflns_Friedel_coverage         0.000
_reflns_number_gt                952
_reflns_number_total             1018
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02016g2.cif
_cod_data_source_block           tb83-rt
_cod_depositor_comments
'Adding full bibliography for 7047316--7047320.cif.'
_cod_database_code               7047318
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.213
_shelx_estimated_absorpt_t_min   0.213
_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. Rigid bond restraints
 C25, C19, C24, C23, C22, C21, C20, C26, C16, C10, C9, C4, C5, C6, C7, C8, C3,
 C2, C1, C13, C28, C27, C17, C12, C11, C29, C18, C30, C15, C14
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3.a Ternary CH refined with riding coordinates:
 N4(H4), N2(H2)
3.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C28(H28A,H28B), C27(H27A,H27B), C12(H12A,H12B), C29(H29A,
 H29B), C14(H14A,H14B)
3.c Aromatic/amide H refined with riding coordinates:
 C23(H23), C22(H22), C21(H21), C20(H20), C26(H26), C5(H5), C6(H6), C7(H7),
 C8(H8), C3(H3), C2(H2A), C17(H17), C11(H11), C18(H18)
3.d Fitted hexagon refined as free rotating group:
 C19(C24,C23,C22,C21,C20), C9(C4,C5,C6,C7,C8)
3.e Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C15(H15A,H15B,H15C)
;
_olex2_submission_special_instructions 'No special instructions were received'