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_7039987
_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         'C20 H20 Fe N12, 2(B F4)'
_chemical_formula_sum            'C20 H20 B2 F8 Fe N12'
_chemical_formula_weight         657.95
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-04-27
_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                 97.843(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.0567(3)
_cell_length_b                   7.6103(2)
_cell_length_c                   17.2769(6)
_cell_measurement_reflns_used    6136
_cell_measurement_temperature    99.95(10)
_cell_measurement_theta_max      73.7170
_cell_measurement_theta_min      4.7870
_cell_volume                     1309.91(7)
_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
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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      99.95(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3756
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
  1 omega -124.00  -79.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3987  -99.0000    0.0000 90

  2 omega -124.00  -79.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3987  -99.0000   90.0000 90

  3 omega -115.00  -12.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3987  -57.0000  -30.0000 206

  4 omega -124.00  -79.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3987  -99.0000   60.0000 90

  5 omega  -71.00   33.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3987   57.0000  120.0000 208

  6 omega    1.00   83.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       41.3987  -99.0000  -90.0000 164

  7 omega   23.00   99.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       41.3987 -125.0000 -120.0000 152

  8 omega   24.00  109.00   0.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878  -94.0000   30.0000 170

  9 omega   34.00   98.00   0.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878  -45.0000    0.0000 128

 10 omega   24.00  109.00   0.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878  -94.0000  -30.0000 170

 11 omega   34.00   98.00   0.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878  -45.0000 -120.0000 128

 12 omega   33.00  122.00   0.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878 -125.0000  150.0000 178

 13 omega   30.00   90.00   0.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878  -30.0000   90.0000 120

 14 omega   30.00   90.00   0.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878  -30.0000  -90.0000 120

 15 omega   30.00   90.00   0.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878  -30.0000  120.0000 120

 16 omega   34.00   98.00   0.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878  -45.0000 -180.0000 128

 17 omega   78.00  178.00   0.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878   30.0000  -60.0000 200

 18 omega   33.00  122.00   0.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878 -125.0000  -60.0000 178

 19 omega   30.00  142.00   0.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878  -77.0000  120.0000 224

 20 omega   25.00  170.00   0.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878  -15.0000  -60.0000 290

 21 omega -124.00  -79.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3987  -99.0000  150.0000 90

 22 omega -124.00  -79.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3987  -99.0000 -150.0000 90

 23 omega -115.00  -12.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3987  -57.0000  150.0000 206

 24 omega -115.00  -12.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3987  -57.0000 -120.0000 206

 25 omega -115.00  -12.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3987  -57.0000   60.0000 206

 26 omega   47.00  178.00   0.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878   15.0000 -150.0000 262

 27 omega   78.00  178.00   0.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878   61.0000  -60.0000 200

 28 omega   47.00  178.00   0.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878   15.0000   90.0000 262

 29 omega   75.00  178.00   0.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878   77.0000 -180.0000 206

 30 omega   78.00  178.00   0.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878   61.0000   90.0000 200

 31 omega   81.00  178.00   0.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878   45.0000 -120.0000 194

 32 omega   78.00  178.00   0.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878   61.0000   60.0000 200

 33 omega   78.00  178.00   0.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878   61.0000  120.0000 200

 34 omega   75.00  178.00   0.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878   77.0000    0.0000 206

 35 omega   78.00  178.00   0.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878   61.0000  -30.0000 200

 36 omega    1.00   83.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       41.3987  -99.0000   30.0000 164
;
_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      -0.0196424000
_diffrn_orient_matrix_UB_12      0.1861738000
_diffrn_orient_matrix_UB_13      0.0315175000
_diffrn_orient_matrix_UB_21      0.0429754000
_diffrn_orient_matrix_UB_22      0.0793181000
_diffrn_orient_matrix_UB_23      -0.0748255000
_diffrn_orient_matrix_UB_31      -0.1472576000
_diffrn_orient_matrix_UB_32      -0.0020781000
_diffrn_orient_matrix_UB_33      -0.0388623000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            5451
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         74.20
_diffrn_reflns_theta_min         4.82
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.490
_exptl_absorpt_correction_T_max  0.921
_exptl_absorpt_correction_T_min  0.520
_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            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.668
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.2926
_exptl_crystal_size_mid          0.0371
_exptl_crystal_size_min          0.0201
_refine_diff_density_max         0.559
_refine_diff_density_min         -0.515
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         5451
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0454
_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^)+(0.0767P)^2^+0.6176P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1233
_refine_ls_wR_factor_ref         0.1257
_reflns_number_gt                4977
_reflns_number_total             5451
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt01898j2.cif
_cod_data_source_block           3_HL_BF4
_cod_depositor_comments
'Adding full bibliography for 7039984--7039987.cif.'
_cod_database_code               7039987
_chemical_oxdiff_formula         'C20 H20 Fe B2 F8'
_diffrn_oxdiff_twin_integration_method simultaneous
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5083(10) 0.4917(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
3. Shared sites
{N3, C8A}
{N3A, C8}
{C7, N5A}
{C7A, N5}
4. Rigid bond restraints
 F1, F2, F3, F4, B1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F1A, F2A, F3A, F4A, B1A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
Uanis(N3) = Uanis(C8A)
Uanis(N3A) = Uanis(C8)
Uanis(C7) = Uanis(N5A)
Uanis(C7A) = Uanis(N5)
6. Same fragment restrains
{F1, F2, F3, F4, B1} sigma for 1-2: 0.02, 1-3: 0.04
as
{F1A, F2A, F3A, F4A, B1A}
7. Others
 Sof(H1B)=Sof(C8A)=Sof(H5B)=Sof(H6B)=Sof(N5A)=Sof(H5AA)=Sof(C7A)=Sof(H7A)=
 Sof(N3A)=Sof(H9B)=Sof(H10A)=1-FVAR(1)
 Sof(H1A)=Sof(N3)=Sof(H5A)=Sof(H6A)=Sof(C7)=Sof(H7)=Sof(N5)=Sof(H5)=Sof(C8)=
 Sof(H9A)=Sof(H10)=FVAR(1)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(F4A)=Sof(B1A)=1-FVAR(2)
 Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=Sof(B1)=FVAR(2)
8.a Ternary CH refined with riding coordinates:
 C1(H1A), C1(H1B)
8.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5A), C5(H5B), C6(H6A), C6(H6B), C7(H7), N5A(H5AA),
  N5(H5), C7A(H7A), C9(H9A), C9(H9B), C10(H10), C10(H10A)
;
_olex2_date_sample_data_collection 2016-04-16
_olex2_date_sample_submission    2016-04-11
_olex2_submission_special_instructions 'No special instructions were received'