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_7039985
_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, 2(B F4), 2(C2 H3 N)'
_chemical_formula_sum            'C38 H38 B2 F8 Fe N14'
_chemical_formula_weight         920.29
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-08-31
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-05-06 deposited with the CCDC.
2016-07-20 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 114.357(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.8095(12)
_cell_length_b                   26.527(3)
_cell_length_c                   9.2849(14)
_cell_measurement_reflns_used    1673
_cell_measurement_temperature    240.00(14)
_cell_measurement_theta_max      51.7000
_cell_measurement_theta_min      4.9240
_cell_volume                     2201.0(6)
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      240.00(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3756
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details
;
  1 omega -115.00  -12.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3987  -57.0000  -90.0000 103

  2 omega -124.00  -79.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3987  -99.0000   60.0000 45

  3 omega  -96.00   -2.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3987  125.0000    0.0000 94

  4 omega    1.00   83.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       41.3987  -99.0000 -120.0000 82

  5 omega   30.00   90.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878  -30.0000  -60.0000 60

  6 omega   81.00  178.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878   45.0000   60.0000 97

  7 omega   78.00  178.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878   30.0000 -150.0000 100

  8 omega   34.00   98.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878  -45.0000   90.0000 64

  9 omega   34.00   98.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878  -45.0000  -60.0000 64

 10 omega   94.00  178.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878  125.0000  -90.0000 84

 11 omega   30.00   90.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878  -30.0000 -120.0000 60

 12 omega   30.00   90.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878  -30.0000   60.0000 60

 13 omega -124.00  -79.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3987  -99.0000    0.0000 45

 14 omega -115.00  -12.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3987  -57.0000   30.0000 103

 15 omega -120.00   -8.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3987  -77.0000  150.0000 112

 16 omega   34.00   98.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878  -45.0000    0.0000 64

 17 omega   47.00  178.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878   15.0000    0.0000 131

 18 omega   78.00  178.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878   61.0000  120.0000 100

 19 omega   81.00  169.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878   45.0000 -120.0000 88

 20 omega   24.00  109.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2878  -94.0000 -120.0000 85
;
_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      -0.1112843000
_diffrn_orient_matrix_UB_12      -0.0430431000
_diffrn_orient_matrix_UB_13      -0.0793984000
_diffrn_orient_matrix_UB_21      -0.0442874000
_diffrn_orient_matrix_UB_22      -0.0011095000
_diffrn_orient_matrix_UB_23      0.1409913000
_diffrn_orient_matrix_UB_31      -0.1241933000
_diffrn_orient_matrix_UB_32      0.0389312000
_diffrn_orient_matrix_UB_33      -0.0834773000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.2025
_diffrn_reflns_av_unetI/netI     0.1245
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            21088
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         74.66
_diffrn_reflns_theta_min         3.33
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.447
_exptl_absorpt_correction_T_max  0.954
_exptl_absorpt_correction_T_min  0.714
_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    1.389
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.4155
_exptl_crystal_size_mid          0.0352
_exptl_crystal_size_min          0.0297
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.794
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         4443
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.2894
_refine_ls_R_factor_gt           0.1643
_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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3850
_refine_ls_wR_factor_ref         0.5049
_reflns_number_gt                1044
_reflns_number_total             4443
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt01898j2.cif
_cod_data_source_block           1_2CH3CN_240K_BnL_BF4
_cod_depositor_comments
'Adding full bibliography for 7039984--7039987.cif.'
_cod_original_cell_volume        2201.0(5)
_cod_database_code               7039985
_chemical_oxdiff_formula         'Fe C34 H32 N12 B2 F8 C4 H6 N2'
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 F3, B1, F2, F1, F4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3.a Ternary CH refined with riding coordinates:
 C10(H10)
3.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B)
3.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C13(H13),
 C14(H14), C15(H15), C16(H16), C17(H17)
3.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C)
;
_olex2_date_sample_data_collection 2015-08-30
_olex2_date_sample_submission    2015-08-24
_olex2_submission_special_instructions 'No special instructions were received'