A Synthetically Tunable System To Control MLCT Excited-State Lifetimes and Spin States in Iron(II) Polypyridines.
Fatur, Steven M.; Shepard, Samuel G.; Higgins, Robert F.; Shores, Matthew P.; Damrauer, Niels H.; Journal of the American Chemical Society 139 (2017) 4493–4505; doi:10.1021/jacs.7b00700

data_4125861
_publ_section_title
;
 A Synthetically Tunable System To Control MLCT Excited-State Lifetimes
 and Spin States in Iron(II) Polypyridines.
;
_journal_issue                   12
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4493
_journal_page_last               4505
_journal_paper_doi               10.1021/jacs.7b00700
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         'C30 H18 F4 Fe N6, 2(B F4), C2 H3 N'
_chemical_formula_sum            'C32 H21 B2 F12 Fe N7'
_chemical_formula_weight         809.03
_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
_audit_creation_date             2016-12-27
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 93.950(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9455(9)
_cell_length_b                   28.393(2)
_cell_length_c                   11.0501(9)
_cell_measurement_reflns_used    9882
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      25.10
_cell_measurement_theta_min      2.81
_cell_volume                     3425.9(5)
_computing_cell_refinement       'Bruker APEX 3'
_computing_data_collection       'Bruker APEX 3'
_computing_data_reduction        'SAINT (Bruker AXS, 2015)'
_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      300.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0746
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            95098
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.341
_diffrn_reflns_theta_min         2.353
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.542
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6617
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0680 before and 0.0604 after correction.
The Ratio of minimum to maximum transmission is 0.8874.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_description       Block
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.376
_exptl_crystal_size_mid          0.305
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.426
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     553
_refine_ls_number_reflns         8508
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1014
_refine_ls_R_factor_gt           0.0569
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0656P)^2^+1.7390P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1297
_refine_ls_wR_factor_ref         0.1527
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5428
_reflns_number_total             8508
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b00700_si_002.cif
_cod_data_source_block           Fedftpy2at300k
_cod_depositor_comments
'Adding full bibliography for 4125861--4125864.cif.'
_cod_database_code               4125861
_shelx_estimated_absorpt_t_max   0.899
_shelx_estimated_absorpt_t_min   0.822
_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. Restrained distances
 F5-B1 \\sim F5A-B1 \\sim F6-B1 \\sim F6A-B1 \\sim F7-B1 \\sim F7A-B1 \\sim
F8-B1 \\sim F8A-B1
 with sigma of 0.002
 F9-B2 \\sim F9A-B2 \\sim F10-B2 \\sim F11-B2 \\sim F11A-B2 \\sim F12-B2 \\sim
F12A-B2
 with sigma of 0.002
3. Others
 Sof(F9A)=Sof(F11A)=Sof(F12A)=1-FVAR(1)
 Sof(F9)=Sof(F11)=Sof(F12)=FVAR(1)
 Sof(F5A)=Sof(F6A)=Sof(F7A)=Sof(F8A)=1-FVAR(2)
 Sof(F5)=Sof(F6)=Sof(F7)=Sof(F8)=FVAR(2)
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C12(H12), C13(H13), C14(H14),
 C17(H17), C18(H18), C19(H19), C22(H22), C23(H23), C24(H24), C27(H27), C28(H28),
  C29(H29)
4.b Idealised Me refined as rotating group:
 C2S(H2SA,H2SB,H2SC)
;
_shelx_res_checksum              46019
_shelx_hkl_checksum              96063
_shelx_shelxl_version_number     2016/4
_olex2_submission_special_instructions 'No special instructions were received'