Mononuclear complexes of a tridentate redox-active ligand with sulfonamido groups: structure, properties, and reactivity.
Cook, Sarah A.; Bogart, Justin A.; Levi, Noam; Weitz, Andrew C.; Moore, Curtis; Rheingold, Arnold L.; Ziller, Joseph W.; Hendrich, Michael P.; Borovik, A. S.; Chemical science 9 (2018) 6540–6547; doi:10.1039/c7sc05445a

data_1549655
_publ_section_title
;
 Mononuclear complexes of a tridentate redox-active ligand with
 sulfonamido groups: structure, properties, and reactivity.
;
_journal_issue                   31
_journal_name_full               'Chemical science'
_journal_page_first              6540
_journal_page_last               6547
_journal_paper_doi               10.1039/c7sc05445a
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         'C52 H62 Fe N5 O4 S2'
_chemical_formula_sum            'C52 H62 Fe N5 O4 S2'
_chemical_formula_weight         941.03
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-09-29
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-12-21 deposited with the CCDC.
2018-07-02 downloaded from the CCDC.
;
_cell_angle_alpha                84.402(6)
_cell_angle_beta                 81.108(7)
_cell_angle_gamma                76.300(7)
_cell_formula_units_Z            2
_cell_length_a                   10.175(2)
_cell_length_b                   16.218(3)
_cell_length_c                   16.588(3)
_cell_measurement_reflns_used    7415
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      24.872
_cell_measurement_theta_min      2.188
_cell_volume                     2622.2(9)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2017)'
_computing_data_collection       'APEX3 v2016.1-0 (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2017)'
_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      100.0
_diffrn_detector                 'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean 8.258
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II Ultra'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Double Bounce Multilayer Mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0702
_diffrn_reflns_av_unetI/netI     0.0773
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            42428
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.641
_diffrn_reflns_theta_min         1.245
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Bruker TXS'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.413
_exptl_absorpt_correction_T_max  0.0265
_exptl_absorpt_correction_T_min  0.0099
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1432 before and 0.0719 after correction. The Ratio of minimum to maximum transmission is 0.3736. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'Bluish Purple'
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_colour_primary    Purple
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_description       Blade
_exptl_crystal_F_000             998
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.396
_refine_diff_density_min         -0.613
_refine_diff_density_rms         0.099
_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     615
_refine_ls_number_reflns         9674
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.1327
_refine_ls_R_factor_gt           0.0961
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0984P)^2^+14.3469P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2401
_refine_ls_wR_factor_ref         0.2653
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6796
_reflns_number_total             9674
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc05445a2.cif
_cod_data_source_block           Boro124
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' 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.

'_exptl_crystal_colour_modifier' value 'Bluish' changed to 'bluish'
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 

 Adding full bibliography for 1549655--1549660.cif.
;
_cod_original_cell_volume        2622.3(10)
_cod_database_code               1549655
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.984
_shelx_estimated_absorpt_t_min   0.922
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9575(17)
 0.0134(9) 0.0168(10) 0.0123(11)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C47B) = Uanis(C47)
4. Rigid body (RIGU) restrains
 C41, C47, C47B, C48, C48B, C49, C49B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Sof(C47B)=Sof(H47B)=Sof(C48B)=Sof(H48D)=Sof(H48E)=Sof(H48F)=Sof(C49B)=
 Sof(H49D)=Sof(H49E)=Sof(H49F)=1-FVAR(1)
 Sof(C47)=Sof(H47)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(H48C)=Sof(C49)=Sof(H49A)=
 Sof(H49B)=Sof(H49C)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C29(H29), C32(H32), C35(H35), C44(H44), C47(H47), C47B(H47B), C50(H50)
6.b Me refined with riding coordinates:
 C49B(H49D,H49E,H49F)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11), C13(H13),
 C14(H14), C15(H15), C16(H16), C19(H19), C20(H20), C21(H21), C22(H22), C25(H25),
  C27(H27), C40(H40), C42(H42)
6.d Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C), C34(H34A,H34B,
 H34C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C45(H45A,H45B,H45C), C46(H46A,
 H46B,H46C), C48(H48A,H48B,H48C), C48B(H48D,H48E,H48F), C49(H49A,H49B,H49C),
 C51(H51A,H51B,H51C), C52(H52A,H52B,H52C)
;
_shelx_res_checksum              93610
_shelx_fab_checksum              77485
_olex2_submission_special_instructions 'No special instructions were received'