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_4125863
_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 Br4 Fe N6, 2(B F4), C4 H10 O'
_chemical_formula_sum            'C34 H28 B2 Br4 F8 Fe N6 O'
_chemical_formula_weight         1085.73
_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
_audit_creation_date             2016-12-28
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 112.8502(19)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.1642(12)
_cell_length_b                   16.9913(10)
_cell_length_c                   23.7983(13)
_cell_measurement_reflns_used    9604
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.63
_cell_measurement_theta_min      2.90
_cell_volume                     7886.4(8)
_computing_cell_refinement       'Bruker Apex 3'
_computing_data_collection       'Bruker Apex 3'
_computing_data_reduction        'Bruker Apex 3'
_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    'ShelXS (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.96
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.989
_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_unetI/netI     0.0303
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19512
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.359
_diffrn_reflns_theta_min         2.636
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.511
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.5774
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0782 before and 0.0534 after correction.
The Ratio of minimum to maximum transmission is 0.7741.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.829
_exptl_crystal_description       Plate
_exptl_crystal_F_000             4240
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         3.721
_refine_diff_density_min         -2.151
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.171
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1069
_refine_ls_number_reflns         19512
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.171
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0570
_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^)+103.3311P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1422
_refine_ls_wR_factor_ref         0.1454
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16988
_reflns_number_total             19512
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b00700_si_005.cif
_cod_data_source_block           fedbtpy2
_cod_depositor_comments
'Adding full bibliography for 4125861--4125864.cif.'
_cod_database_code               4125863
_shelx_estimated_absorpt_t_max   0.345
_shelx_estimated_absorpt_t_min   0.266
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.8955(14) 0.1045(14)
2. 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, All C(H,H,H,H,H,H) groups
3. Uiso/Uaniso restraints and constraints
C27 \\sim C28 \\sim C29: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002
4. Others
 Sof(O3)=Sof(H31D)=Sof(H31E)=Sof(H31F)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(C40)=
 Sof(H40A)=Sof(H40B)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=1-FVAR(1)
 Sof(O1)=Sof(H31A)=Sof(H31B)=Sof(H31C)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(C33)=
 Sof(H33A)=Sof(H33B)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=FVAR(1)
 Sof(O4)=Sof(H38D)=Sof(H38E)=Sof(H38F)=Sof(C42)=Sof(H42A)=Sof(H42B)=1-FVAR(2)
 Sof(O2)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(H38A)=Sof(H38B)=Sof(H38C)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C33(H33A,H33B), C39(H39A,H39B), C40(H40A,H40B), C36(H36A,
 H36B), C37(H37A,H37B), C42(H42A,H42B)
5.b Me refined with riding coordinates:
 C31(H31A,H31B,H31C), C31(H31D,H31E,H31F), C38(H38A,H38B,H38C), C38(H38D,H38E,
 H38F)
5.c 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), 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')
5.d Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C41(H41A,H41B,H41C), C35(H35A,H35B,H35C)
;
_shelx_res_checksum              96772
_shelx_hkl_checksum              6553
_shelx_shelxl_version_number     2016/4
_olex2_submission_special_instructions 'No special instructions were received'