Accessing spin-crossover behaviour in iron(ii) complexes of N-confused scorpionate ligands.
Gardinier, James R.; Treleven, Alex R.; Meise, Kristin J.; Lindeman, Sergey V.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 12639–12643; doi:10.1039/c6dt01898j

data_7039986
_publ_section_title
;
 Accessing spin-crossover behaviour in iron(ii) complexes of N-confused
 scorpionate ligands.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12639
_journal_page_last               12643
_journal_paper_doi               10.1039/c6dt01898j
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety
'C34 H32 Fe N12 O4 S2, B F4, 2(B0.5 F1.37), 2(C2 H3 N), 1.26(F)'
_chemical_formula_sum            'C38 H38 B2 F8 Fe N14 O4 S2'
_chemical_formula_weight         1048.41
_chemical_name_systematic
;
 ? 
;
_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   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-02-22
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-07-14 deposited with the CCDC.
2016-07-20 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 93.3163(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.4741(4)
_cell_length_b                   17.7632(3)
_cell_length_c                   10.49352(18)
_cell_measurement_reflns_used    10831
_cell_measurement_temperature    99.8(4)
_cell_measurement_theta_max      29.2190
_cell_measurement_theta_min      2.8910
_cell_volume                     4368.21(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.8(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3756
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.909
_diffrn_measurement_details
;
  1 omega -100.00  -55.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.5916  178.0000   30.0000 45

  2 omega  -20.00   30.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.5916  -99.0000  150.0000 50

  3 omega   34.00  100.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       11.6697 -178.0000  120.0000 66

  4 omega  -35.00   93.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       11.6697   19.0000 -150.0000 128

  5 omega  -88.00   15.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.5916  -37.0000 -120.0000 103

  6 omega  -64.00  -25.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       11.6697  -37.0000 -180.0000 39
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0022449000
_diffrn_orient_matrix_UB_12      -0.0233651000
_diffrn_orient_matrix_UB_13      -0.0548882000
_diffrn_orient_matrix_UB_21      -0.0264026000
_diffrn_orient_matrix_UB_22      -0.0141520000
_diffrn_orient_matrix_UB_23      0.0193404000
_diffrn_orient_matrix_UB_31      -0.0146168000
_diffrn_orient_matrix_UB_32      0.0291371000
_diffrn_orient_matrix_UB_33      -0.0345972000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_unetI/netI     0.0309
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            24870
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         29.45
_diffrn_reflns_theta_min         2.85
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.535
_exptl_absorpt_correction_T_max  0.932
_exptl_absorpt_correction_T_min  0.828
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.5237
_exptl_crystal_size_mid          0.3004
_exptl_crystal_size_min          0.1559
_refine_diff_density_max         0.520
_refine_diff_density_min         -0.524
_refine_diff_density_rms         0.065
_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     342
_refine_ls_number_reflns         5524
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0390
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0348P)^2^+8.5278P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0860
_refine_ls_wR_factor_ref         0.0949
_reflns_number_gt                4575
_reflns_number_total             5524
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt01898j2.cif
_cod_data_source_block           2_2CH3CN_TsL_BF4
_cod_depositor_comments
'Adding full bibliography for 7039984--7039987.cif.'
_cod_database_code               7039986
_chemical_oxdiff_formula         'C34 H32 N12 S2 O4 Fe B2 F8 C H3 N'
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uiso(N7) = Uiso(N7A)
Uiso(F4) = Uiso(F7) = Uiso(F3)
3. Same fragment restrains
{N7, C18, C19} sigma for 1-2: 0.02, 1-3: 0.04
as
{N7A, C18A, C19A}
4. Others
 Sof(N7A)=Sof(C18A)=Sof(C19A)=Sof(H19D)=Sof(H19E)=Sof(H19F)=1-FVAR(1)
 Sof(N7)=Sof(C18)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=FVAR(1)
 Sof(F7)=1-FVAR(2)
 Sof(F8)=Sof(F9)=0.5*(1-FVAR(3))
 Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=0.5*FVAR(3)
 Fixed Sof: B2(0.5)
5.a Ternary CH refined with riding coordinates:
 C1(H1)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C12(H12),
 C13(H13), C15(H15), C16(H16)
5.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C19A(H19D,H19E,H19F)
;
_olex2_date_sample_data_collection 2016-02-20
_olex2_date_sample_submission    2016-02-19
_olex2_submission_special_instructions 'No special instructions were received'