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_7047319
_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         'C30 H34 Fe N4 O2, 0.5(H2 O), Br'
_chemical_formula_sum            'C30 H35 Br Fe N4 O2.5'
_chemical_formula_weight         627.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-11-17
_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                 97.514(7)
_cell_angle_gamma                90
_cell_formula_units_Z            24
_cell_length_a                   46.308(4)
_cell_length_b                   20.8116(15)
_cell_length_c                   19.6811(17)
_cell_measurement_temperature    293
_cell_measurement_theta_max      50
_cell_measurement_theta_min      3.2
_cell_volume                     18805(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 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'Image plate'
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Rigaku Spider'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  'Rigaku VariMax-HF Confocal Optical System'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0989
_diffrn_reflns_av_unetI/netI     0.0914
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            16881
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        33.412
_diffrn_reflns_theta_max         33.412
_diffrn_reflns_theta_min         5.554
_diffrn_source                   'Rigaku MM007 rotating anode'
_exptl_absorpt_coefficient_mu    5.612
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.484
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_density_meas      ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             7776
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.444
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.006
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     886
_refine_ls_number_reflns         3540
_refine_ls_number_restraints     663
_refine_ls_restrained_S_all      1.840
_refine_ls_R_factor_all          0.2470
_refine_ls_R_factor_gt           0.1631
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3696
_refine_ls_wR_factor_ref         0.4112
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1215
_reflns_number_total             3540
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02016g2.cif
_cod_data_source_block           tb67rt3-2m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/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.

'_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_formula_sum        'C30 H35 Br Fe N4 O2.50'
_cod_database_code               7047319
_shelx_shelxl_version_number     2014/7
_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
 C45-C44 \\sim C60-C59 \\sim C30-C29 \\sim C15-C14 \\sim C75-C74 \\sim C90-C89
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(N11) \\sim
Ueq, Uanis(C2) \\sim Ueq, Uanis(N10) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(N7)
\\sim Ueq, Uanis(N12) \\sim Ueq, Uanis(N9) \\sim Ueq, Uanis(N8) \\sim Ueq: with
sigma of 0.05 and sigma for terminal atoms of 0.1
: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(N6) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(N2) \\sim
Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C65) \\sim Ueq: with sigma of 0.0005 and sigma for terminal atoms of 0.001
Uanis(C72) \\sim Ueq: with sigma of 0.0005 and sigma for terminal atoms of 0.001
Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O6) \\sim
Ueq, Uanis(O3) \\sim Ueq, Uanis(O4) \\sim Ueq, : with sigma of 0.1 and sigma
for terminal atoms of 0.2
Uanis(N1) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(N4) \\sim
Ueq, Uanis(N9) \\sim Ueq, Uanis(N10) \\sim Ueq, Uanis(N11) \\sim Ueq,
Uanis(N12) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(N7) \\sim
Ueq, Uanis(N8) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C12) \\sim Ueq: with sigma of 0.0005 and sigma for terminal atoms of 0.001
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8)
\\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq,
Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15)
\\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq,
Uanis(C19) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C22)
\\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C25) \\sim Ueq,
Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C29)
\\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(C62) \\sim Ueq,
Uanis(C63) \\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C66)
\\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(C69) \\sim Ueq,
Uanis(C70) \\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(C72) \\sim Ueq, Uanis(C73)
\\sim Ueq, Uanis(C74) \\sim Ueq, Uanis(C75) \\sim Ueq, Uanis(C76) \\sim Ueq,
Uanis(C77) \\sim Ueq, Uanis(C78) \\sim Ueq, Uanis(C79) \\sim Ueq, Uanis(C80)
\\sim Ueq, Uanis(C81) \\sim Ueq, Uanis(C82) \\sim Ueq, Uanis(C83) \\sim Ueq,
Uanis(C84) \\sim Ueq, Uanis(C85) \\sim Ueq, Uanis(C86) \\sim Ueq, Uanis(C87)
\\sim Ueq, Uanis(C88) \\sim Ueq, Uanis(C89) \\sim Ueq, Uanis(C90) \\sim Ueq,
Uanis(C31) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C34)
\\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C37) \\sim Ueq,
Uanis(C38) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C41)
\\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C44) \\sim Ueq,
Uanis(C45) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C48)
\\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C51) \\sim Ueq,
Uanis(C52) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C55)
\\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C58) \\sim Ueq,
Uanis(C59) \\sim Ueq, Uanis(C60) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Fixed Sof: O1W(0.5) H1WA(0.5) H1WB(0.5) O2W(0.5) H2WA(0.5) H2WB(0.5) O3W(0.5)
 H3WA(0.5) H3WB(0.5)
 Fixed Uiso: O1W(0.2) H1WA(0.3) H1WB(0.3) O2W(0.2) H2WA(0.3) H2WB(0.3)
 O3W(0.2) H3WA(0.3) H3WB(0.3)
 Fixed X: O1W(0.64454) H1WA(0.63527) H1WB(0.63329) O2W(0.68752) H2WA(0.677)
 H2WB(0.678) O3W(0.5179) H3WA(0.532) H3WB(0.50081)
 Fixed Y: O1W(0.44088) H1WA(0.42798) H1WB(0.463381) O2W(0.579599)
 H2WA(0.617001) H2WB(0.541) O3W(0.91928) H3WA(0.91678) H3WB(0.902609)
 Fixed Z: O1W(0.48319) H1WA(0.515221) H1WB(0.454969) O2W(0.847449) H2WA(0.85)
 H2WB(0.845) O3W(0.64367) H3WA(0.67922) H3WB(0.65309)
5.a Ternary CH refined with riding coordinates:
 N2(H2), N4(H4), N10(H10A), N12(H12), N6(H6), N8(H8A)
5.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C27(H27A,H27B), C28(H28A,
 H28B), C29(H29A,H29B), C72(H72A,H72B), C73(H73A,H73B), C74(H74A,H74B),
 C87(H87A,H87B), C88(H88A,H88B), C89(H89A,H89B), C42(H42A,H42B), C43(H43A,H43B),
  C44(H44A,H44B), C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B)
5.c Me refined with riding coordinates:
 C15(H15A,H15B,H15C), C30(H30A,H30B,H30C), C75(H75A,H75B,H75C)
5.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4A), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C18(H18),
 C19(H19), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C63(H63), C64(H64),
  C67(H67), C68(H68), C69(H69), C70(H70), C71(H71), C78(H78), C79(H79),
 C82(H82), C83(H83), C84(H84), C85(H85), C86(H86), C33(H33), C34(H34), C37(H37),
  C38(H38), C39(H39), C40(H40), C41(H41), C48(H48), C49(H49), C52(H52),
 C53(H53), C54(H54), C55(H55), C56(H56)
5.e Naphthalene refined as free rotating group:
 C1(C2,C3,C4,C5,C6,C7,C8,C9,C10), C16(C17,C18,C19,C20,C21,C22,C23,C24,C25),
 C61(C62,C63,C64,C65,C66,C67,C68,C69,C70), C76(C77,C78,C79,C80,C81,C82,C83,C84,
 C85), C31(C32,C33,C34,C35,C36,C37,C38,C39,C40), C46(C47,C48,C49,C50,C51,C52,
 C53,C54,C55)
5.f Idealised Me refined as rotating group:
 C90(H90A,H90B,H90C), C45(H45A,H45B,H45C), C60(H60A,H60B,H60C)
;
_olex2_submission_special_instructions 'No special instructions were received'