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_7047320
_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         'Br, C30 H34 Fe N4 O2, H2 O'
_chemical_formula_sum            'C30 H36 Br Fe N4 O3'
_chemical_formula_weight         636.39
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-08-11
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2018-08-17 deposited with the CCDC.
2018-08-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.188(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.551(5)
_cell_length_b                   20.824(5)
_cell_length_c                   15.874(4)
_cell_measurement_reflns_used    1023
_cell_measurement_temperature    103
_cell_measurement_theta_max      40.2
_cell_measurement_theta_min      4.2
_cell_volume                     6174(3)
_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-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      103
_diffrn_detector                 'Image plate'
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
scan:
    Number of images: 40
               Slice: 20.0000 - 220.0000
         Image width: 5.0000
            Exp time: 180.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 0.0000
                 XTD: 127.4000
              2theta: 0.0000
scan:
    Number of images: 38
               Slice: 22.0000 - 212.0000
         Image width: 5.0000
            Exp time: 180.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 90.0000
                 XTD: 127.4000
              2theta: 0.0000
scan:
    Number of images: 25
               Slice: 51.0000 - 176.0000
         Image width: 5.0000
            Exp time: 180.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 180.0000
                 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      0.014953
_diffrn_orient_matrix_UB_12      -0.025250
_diffrn_orient_matrix_UB_13      0.045519
_diffrn_orient_matrix_UB_21      0.027167
_diffrn_orient_matrix_UB_22      0.039115
_diffrn_orient_matrix_UB_23      0.027409
_diffrn_orient_matrix_UB_31      -0.058195
_diffrn_orient_matrix_UB_32      0.011772
_diffrn_orient_matrix_UB_33      0.006565
_diffrn_radiation_monochromator  'Rigaku VariMax-HF Confocal Optical System'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1523
_diffrn_reflns_av_unetI/netI     0.1449
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            36184
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        58.930
_diffrn_reflns_theta_max         58.930
_diffrn_reflns_theta_min         2.365
_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    5.717
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.225
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2632
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.974
_refine_diff_density_min         -1.117
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     697
_refine_ls_number_reflns         8792
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.1216
_refine_ls_R_factor_gt           0.0968
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2187
_refine_ls_wR_factor_ref         0.2528
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5396
_reflns_number_total             8792
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02016g2.cif
_cod_data_source_block           tb67LT
_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_database_code               7047320
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.658
_shelx_estimated_absorpt_t_min   0.162
_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, All O(H,H) groups
2. Others
 Fixed X: H5A(0.14293) H5B(0.1822) H6A(0.304629) H6B(0.239569)
 Fixed Y: H5A(0.40086) H5B(0.38493) H6A(0.415569) H6B(0.435619)
 Fixed Z: H5A(0.358991) H5B(0.444549) H6A(0.54725) H6B(0.55672)
3.a Ternary CH refined with riding coordinates:
 N2(H2), N22(H22A), N4(H4), N0AA(H0AA)
3.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C12(H12A,H12B), C43(H43A,H43B), C27(H27A,H27B), C58(H58A,
 H58B), C14(H14A,H14B), C28(H28A,H28B), C57(H57A,H57B), C42(H42A,H42B),
 C29(H29A,H29B), C59(H59A,H59B), C44(H44A,H44B)
3.c Aromatic/amide H refined with riding coordinates:
 C64(H64), C17(H17), C2(H2A), C32(H32), C10(H10), C40(H40), C25(H25), C18(H18),
  C41(H41), C56(H56), C3(H3), C9(H9), C24(H24), C33(H33), C55(H55), C8(H8),
 C7(H7), C37(H37), C11(H11), C39(H39), C54(H54), C23(H23), C47(H47), C52(H52),
 C22(H22), C53(H53), C38(H38), C48(H48)
3.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C30(H30A,H30B,H30C), C60(H60A,H60B,H60C), C45(H45A,H45B,
 H45C)
;
_olex2_submission_special_instructions 'No special instructions were received'