Varied spin crossover behaviour in a family of dinuclear Fe(ii) triple helicate complexes.
Archer, Rosanna J.; Scott, Hayley S.; Polson, Matthew I. J.; Williamson, Bryce E.; Mathonière, Corine; Rouzières, Mathieu; Clérac, Rodolphe; Kruger, Paul E.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 7965–7974; doi:10.1039/c8dt01567h

data_7046460
_publ_section_title
;
 Varied spin crossover behaviour in a family of dinuclear Fe(ii) triple
 helicate complexes.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7965
_journal_page_last               7974
_journal_paper_doi               10.1039/c8dt01567h
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety
'C84 H72 Fe2 N18, C H Cl3, O, 2(C2 H3 N), 4(B F4)'
_chemical_formula_sum            'C89 H79 B4 Cl3 F16 Fe2 N20 O'
_chemical_formula_weight         2010.01
_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
_audit_creation_date             2018-05-11
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2018-05-10 deposited with the CCDC.
2018-05-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.960(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.8736(8)
_cell_length_b                   28.1738(6)
_cell_length_c                   14.1358(3)
_cell_measurement_reflns_used    6897
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.6688
_cell_measurement_theta_min      3.1345
_cell_volume                     10064.1(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_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      120(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0507
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            19623
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.832
_diffrn_reflns_theta_min         3.137
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.763
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71199
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic pale green'
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_description       block
_exptl_crystal_F_000             4112
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.022
_refine_diff_density_min         -0.695
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     699
_refine_ls_number_reflns         9886
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0963
_refine_ls_R_factor_gt           0.0806
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1673P)^2^+22.7045P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2326
_refine_ls_wR_factor_ref         0.2501
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7851
_reflns_number_total             9886
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01567h2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7046459--7046462.cif.'
_cod_database_code               7046460
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H14A,H14B,H14C} of C14
 At 1.5 times of:
  {H43A,H43B,H43C} of C43, {H44A,H44B,H44C} of C44, {H17A,H17B,H17C} of C17,
  {H15A,H15B,H15C} of C15
2. Restrained distances
 Cl2-C46 = C46-Cl1 = C46-Cl3
 1.78412 with sigma of 0.02
3. Others
 Fixed Sof: Cl1(0.5) Cl2(0.5) Cl3(0.5) O1(0.5) C46(0.5) H46(0.5) C13(0.5)
 C13A(0.5) C14(0.5) H14A(0.5) H14B(0.5) H14C(0.5) C15(0.5) H15A(0.5) H15B(0.5)
 H15C(0.5) F1(0.75) F2(0.75) F3(0.75) F4(0.75) B1(0.75) F1A(0.25) F3A(0.25)
 F2A(0.25) F4A(0.25) B1A(0.25)
4.a Riding coordinates:
 C14(H14A,H14B,H14C)
4.b Ternary CH refined with riding coordinates:
 C46(H46)
4.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C6(H6), C8(H8), C9(H9), C10(H10), C12(H12),
 C19(H19), C20(H20), C21(H21), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28),
  C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C35(H35), C37(H37),
 C39(H39), C40(H40), C41(H41)
4.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C43(H43A,H43B,H43C), C44(H44A,H44B,
 H44C)
;
_olex2_submission_special_instructions 'No special instructions were received'