Insights into the excited state dynamics of Fe(ii) polypyridyl complexes from variable-temperature ultrafast spectroscopy
Carey, Monica C.; Adelman, Sara L.; McCusker, James K.; Chemical Science  (2019) –; doi:10.1039/C8SC04025G

data_1550339
_publ_section_title
;
 Insights into the excited state dynamics of Fe(ii) polypyridyl complexes
 from variable-temperature ultrafast spectroscopy
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C8SC04025G
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C30 H22 Fe N6, 2(F6 P), 2(C2 H3 N)'
_chemical_formula_sum            'C34 H28 F12 Fe N8 P2'
_chemical_formula_weight         894.43
_space_group_crystal_system      tetragonal
_space_group_IT_number           76
_space_group_name_Hall           'P 4w'
_space_group_name_H-M_alt        'P 41'
_symmetry_space_group_name_Hall  'P 4w'
_symmetry_space_group_name_H-M   'P 41'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-11-06
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-12-12 deposited with the CCDC.
2018-11-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.3462(2)
_cell_length_b                   12.3462(2)
_cell_length_c                   48.9067(9)
_cell_measurement_reflns_used    9956
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      72.15
_cell_measurement_theta_min      4.01
_cell_volume                     7454.8(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'COSMO (BRUKER, V1.61, 2009)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
'SHELXL (Sheldrick, Acta Cryst. A64 2008, 112-122)'
_computing_structure_solution
'SHELXS (Sheldrick, Acta Cryst. A64 2008, 112-122)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 8.4
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_unetI/netI     0.0912
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       60
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            26729
_diffrn_reflns_point_group_measured_fraction_full 0.826
_diffrn_reflns_point_group_measured_fraction_max 0.811
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.144
_diffrn_reflns_theta_min         3.615
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.957
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.6018
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0986 before and 0.0747 after correction. The Ratio of minimum to maximum transmission is 0.7986. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_description       plate
_exptl_crystal_F_000             3616
_exptl_crystal_size_max          0.216
_exptl_crystal_size_mid          0.193
_exptl_crystal_size_min          0.159
_refine_diff_density_max         0.518
_refine_diff_density_min         -0.379
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details
;
 Flack x determined using 3167 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.016(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1031
_refine_ls_number_reflns         11934
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0487
_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^)+(0.0369P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1081
_refine_ls_wR_factor_ref         0.1141
_reflns_Friedel_coverage         0.617
_reflns_Friedel_fraction_full    0.653
_reflns_Friedel_fraction_max     0.627
_reflns_number_gt                9923
_reflns_number_total             11934
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc04025g2.cif
_cod_data_source_block           sla_terpy_1
_cod_original_cell_volume        7454.8(3)
_cod_database_code               1550339
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.506
_shelx_estimated_absorpt_t_min   0.414
_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.a Aromatic/amide H refined with riding coordinates:
 C00M(H00M), C00S(H00S), C00Y(H00Y), C00Z(H00Z), C017(H017), C01A(H01A),
 C01B(H01B), C01C(H01C), C01D(H01D), C01E(H01E), C01H(H01H), C01I(H01I),
 C01J(H01J), C01K(H01K), C01L(H01L), C01M(H01M), C01O(H01O), C01Q(H01Q),
 C01R(H01R), C01T(H01T), C01V(H01V), C01X(H01X), C01Y(H01Y), C01Z(H01Z),
 C020(H020), C021(H021), C023(H023), C025(H025), C026(H026), C027(H027),
 C028(H028), C029(H029), C02A(H02A), C02B(H02B), C02G(H02G), C02H(H02H),
 C02J(H02J), C02K(H02K), C02N(H02N), C02Q(H02Q), C02R(H02R), C02U(H02U),
 C02W(H02W), C030(H030)
2.b Idealised Me refined as rotating group:
 C02T(H02C,H02D,H02E), C02X(H02F,H02I,H02L), C032(H03A,H03B,H03C), C1(H1A,H1B,
 H1C)
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a nylon loop with paratone oil'
_olex2_submission_original_sample_id SLA_terpy
_olex2_submission_special_instructions 'No special instructions were received'