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_1550340
_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_formula_moiety         'C36 H36 Fe N6, 2(F6 P), C4 H9 O'
_chemical_formula_sum            'C40 H45 F12 Fe N6 O P2'
_chemical_formula_weight         971.61
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-11-13
_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                83.227(2)
_cell_angle_beta                 85.655(2)
_cell_angle_gamma                82.022(2)
_cell_formula_units_Z            2
_cell_length_a                   8.6648(2)
_cell_length_b                   14.3856(3)
_cell_length_c                   17.4683(4)
_cell_measurement_reflns_used    3493
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      69.96
_cell_measurement_theta_min      2.55
_cell_volume                     2137.36(8)
_computing_cell_refinement       'APEX2 (BRUKER, V2012.10-0, 2012)'
_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 0.965
_diffrn_measured_fraction_theta_max 0.960
_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  0.1207
_diffrn_reflns_av_unetI/netI     0.0958
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25863
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.108
_diffrn_reflns_theta_min         2.552
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.370
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.5575
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0798 before and 0.0649 after correction. The Ratio of minimum to maximum transmission is 0.7401. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_description       Needle
_exptl_crystal_F_000             998
_exptl_crystal_size_max          0.199
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.054
_refine_diff_density_max         0.480
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     567
_refine_ls_number_reflns         7808
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1102
_refine_ls_R_factor_gt           0.0625
_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^)+(0.0705P)^2^+0.7151P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1410
_refine_ls_wR_factor_ref         0.1643
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4993
_reflns_number_total             7808
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc04025g2.cif
_cod_data_source_block           sla2079_meoh_1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               1550340
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.798
_shelx_estimated_absorpt_t_min   0.477
_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.a Secondary CH2 refined with riding coordinates:
 C38(H38A,H38B)
2.b Aromatic/amide H refined with riding coordinates:
 C31(H31), C28(H28), C10(H10), C25(H25), C19(H19), C1(H1), C2(H2), C34(H34),
 C21(H21), C4(H4), C9(H9), C16(H16), C22(H22), C7(H7), C13(H13), C33(H33),
 C26(H26), C14(H14), C39(H39)
2.c Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C11(H11A,H11B,H11C), C35(H35A,H35B,H35C), C24(H24A,H24B,
 H24C), C23(H23A,H23B,H23C), C12(H12A,H12B,H12C), C37(H37A,H37B,H37C), C40(H40A,
 H40B,H40C)
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'