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_7047316
_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         '2(C30 H34 Fe N4 O2), 2(Cl), 2(O)'
_chemical_formula_sum            'C30 H36 Cl Fe N4 O3'
_chemical_formula_weight         591.94
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2017-05-30
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2018-08-17 deposited with the CCDC.
2018-08-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.500(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.4013(19)
_cell_length_b                   20.567(2)
_cell_length_c                   16.0495(17)
_cell_measurement_reflns_used    4911
_cell_measurement_temperature    293
_cell_measurement_theta_max      50.4
_cell_measurement_theta_min      2.4
_cell_volume                     6140.5(11)
_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    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'Image plate'
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
scan:
    Number of images: 62
               Slice: 21.0000 - 176.0000
         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: 72
               Slice: 20.0000 - 200.0000
         Image width: 2.5000
            Exp time: 60.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 0.0000
                 Phi: 0.0000
                 XTD: 127.4000
              2theta: 0.0000
scan:
    Number of images: 48
               Slice: 50.0000 - 170.0000
         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
scan:
    Number of images: 68
               Slice: 24.0000 - 194.0000
         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: 36
               Slice: 87.0000 - 177.0000
         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
;
_diffrn_measurement_device
;
Crystal Goniometer
;
_diffrn_measurement_device_type  'Rigaku Spider'
_diffrn_measurement_method       \w-scans
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       FS_PROCESS
_diffrn_orient_matrix_UB_11      -0.013830
_diffrn_orient_matrix_UB_12      -0.046247
_diffrn_orient_matrix_UB_13      -0.014776
_diffrn_orient_matrix_UB_21      -0.000906
_diffrn_orient_matrix_UB_22      0.011271
_diffrn_orient_matrix_UB_23      -0.050347
_diffrn_orient_matrix_UB_31      0.063488
_diffrn_orient_matrix_UB_32      -0.009913
_diffrn_orient_matrix_UB_33      0.011691
_diffrn_radiation_monochromator  'Rigaku VariMax-HF Confocal Optical System'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1125
_diffrn_reflns_av_unetI/netI     0.1256
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            37060
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        50.4
_diffrn_reflns_theta_max         50.4
_diffrn_reflns_theta_min         2.2
_diffrn_source                   'Rigaku MM007 rotating anode'
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.024
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.370
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2488
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.801
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     707
_refine_ls_number_reflns         6388
_refine_ls_number_restraints     121
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.1946
_refine_ls_R_factor_gt           0.0982
_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^)+(0.1487P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2237
_refine_ls_wR_factor_ref         0.2708
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3159
_reflns_number_total             6388
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02016g2.cif
_cod_data_source_block           tb65_rt
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7047316--7047320.cif.
;
_cod_original_cell_volume        6140.4(11)
_cod_database_code               7047316
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.689
_shelx_estimated_absorpt_t_min   0.482
_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. Restrained distances
 Cl2-O5 \\sim Cl1-O6
 with sigma of 0.02
3. Rigid bond restraints
 C6, C21, C36, C4, C1, C5, C12, C35, C2, C10, C26, C56, C31, C11, C34, C40,
 C39, C41, C51, C32, C50, C17, C16, C14, C18, C20, C29, C7, C9, C25, C24, C46,
 C8, C13, C27, C19, C42, C33, C37, C3, C28, C55, C23, C59, C22, C49, C43, C15,
 C44, C54, C58, C53, C48, C52, C38, C47, C57, C60, C45, C30
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4.a Ternary CH refined with riding coordinates:
 N8(H8A), N4(H4), N2(H2), N6(H6)
4.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C14(H14A,H14B), C29(H29A,H29B), C13(H13A,H13B), C27(H27A,
 H27B), C42(H42A,H42B), C28(H28A,H28B), C59(H59A,H59B), C43(H43A,H43B),
 C44(H44A,H44B), C58(H58A,H58B), C57(H57A,H57B)
4.c Aromatic/amide H refined with riding coordinates:
 C2(H2A), C10(H10), C26(H26), C56(H56), C11(H11), C40(H40), C39(H39), C41(H41),
  C32(H32), C17(H17), C18(H18), C7(H7), C9(H9), C25(H25), C24(H24), C8(H8),
 C33(H33), C37(H37), C3(H3), C55(H55), C23(H23), C22(H22), C54(H54), C53(H53),
 C48(H48), C52(H52), C38(H38), C47(H47)
4.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C60(H60A,H60B,H60C), C45(H45A,H45B,H45C), C30(H30A,H30B,
 H30C)
;
_shelx_res_checksum              86168
_olex2_submission_special_instructions 'No special instructions were received'