Electrochemical behaviors of a pincer-type NNN-Fe complex and catalytic H<sub>2</sub> evolution activity.
Song, Seungjin; Lee, Junseong; Choi, Jun-Ho; Seo, Junhyeok; Chemical communications (Cambridge, England) 57 (2021) 7497–7500; doi:10.1039/d1cc03050g

data_7128588
_publ_section_title
;
 Electrochemical behaviors of a pincer-type NNN-Fe complex and catalytic
 H<sub>2</sub> evolution activity.
;
_journal_issue                   61
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              7497
_journal_page_last               7500
_journal_paper_doi               10.1039/d1cc03050g
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C32 H56 Fe N8, 2(Cl O4), C2 H3.001 N1'
_chemical_formula_sum            'C34 H59 Cl2 Fe N9 O8'
_chemical_formula_weight         848.65
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2021-01-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-05-12 deposited with the CCDC.	2021-07-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.5619(4)
_cell_length_b                   16.3532(4)
_cell_length_c                   39.3827(9)
_cell_measurement_reflns_used    4037
_cell_measurement_temperature    100
_cell_measurement_theta_max      23.043
_cell_measurement_theta_min      3.67
_cell_volume                     8734.3(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'XS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_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  0.1747
_diffrn_reflns_av_unetI/netI     0.0778
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            117724
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.788
_diffrn_reflns_theta_min         3.088
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.523
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6472
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction.
wR2(int) was 0.0904 before and 0.0723 after correction.
The Ratio of minimum to maximum transmission is 0.8684.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_description       block
_exptl_crystal_F_000             3600
_refine_diff_density_max         0.655
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     563
_refine_ls_number_reflns         8335
_refine_ls_number_restraints     170
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.1158
_refine_ls_R_factor_gt           0.0570
_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^)+(0.0615P)^2^+9.9646P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1251
_refine_ls_wR_factor_ref         0.1541
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5035
_reflns_number_total             8335
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc03050g2.cif
_cod_data_source_block           jsh09-1
_cod_depositor_comments          'Adding full bibliography for 7128588.cif.'
_cod_database_code               7128588
_shelxl_version_number           2014-3
_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, All C(H,H,H,H,H,H) groups
2. Restrained distances
 Cl2A-O8A = Cl2A-O6A = Cl2A-O5A = Cl2A-O7A
 1.5 with sigma of 0.02
 Cl2B-O6B = Cl2B-O7B = Cl2B-O8B = Cl2B-O5B
 1.5 with sigma of 0.02
 Cl2A-O8A \\sim Cl2A-O6A \\sim Cl2A-O5A \\sim Cl2A-O7A
 with sigma of 0.02
 O8A-O5A \\sim O6A-O7A \\sim O8A-O7A \\sim O6A-O5A \\sim O8A-O6A \\sim O5A-O7A
 with sigma of 0.04
 Cl2B-O6B \\sim Cl2B-O7B \\sim Cl2B-O8B \\sim Cl2B-O5B
 with sigma of 0.02
 O6B-O8B \\sim O7B-O5B \\sim O6B-O5B \\sim O7B-O8B \\sim O6B-O7B \\sim O8B-O5B
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Cl2A \\sim O5A \\sim O6A \\sim O7A \\sim O8A: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
Cl2B \\sim O5B \\sim O6B \\sim O7B \\sim O8B: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
Uanis(C34B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 Cl2A, O5A, O6A, O7A, O8A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl2B, O5B, O6B, O7B, O8B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(Cl2B)=Sof(O5B)=Sof(O6B)=Sof(O7B)=Sof(O8B)=1-FVAR(1)
 Sof(Cl2A)=Sof(O5A)=Sof(O6A)=Sof(O7A)=Sof(O8A)=FVAR(1)
 Fixed Sof: H33A(0.667) H33B(0.667) H33C(0.667) H33D(0.33333) H33E(0.33333)
 H33F(0.33333) N9A(0.667) C34A(0.667) N9B(0.33333) C34B(0.33333)
6.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C12(H12A,
 H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4)
6.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C17(H17A,H17B,H17C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C),
 C33(H33A,H33B,H33C), C33(H33D,H33E,H33F)
;
_shelx_res_checksum              63089
_olex2_submission_special_instructions 'No special instructions were received'