A Redox-Switchable, Allosteric Coordination Complex.
Cheng, Ho Fung; d'Aquino, Andrea I; Barroso-Flores, Joaquín; Mirkin, Chad A.; Journal of the American Chemical Society 140 (2018) 14590–14594; doi:10.1021/jacs.8b09321

data_4133287
_publ_section_title
;
 A Redox-Switchable, Allosteric Coordination Complex.
;
_journal_issue                   44
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14590
_journal_page_last               14594
_journal_paper_doi               10.1021/jacs.8b09321
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C20 H20 Cl2 Fe N2 Pt S, C2 H4 Cl2'
_chemical_formula_sum            'C22 H24 Cl4 Fe N2 Pt S'
_chemical_formula_weight         741.23
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-03-07
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 99.06(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.862(4)
_cell_length_b                   9.0804(18)
_cell_length_c                   15.254(3)
_cell_measurement_reflns_used    9253
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.673
_cell_measurement_theta_min      2.529
_cell_volume                     2443.2(9)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'APEX2 V2014.11-0 (Bruker, 2014)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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      99.94
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'QuazarTM optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0520
_diffrn_reflns_av_unetI/netI     0.0505
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            31961
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.669
_diffrn_reflns_theta_min         2.309
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    6.850
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.5313
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1035 before and 0.0554 after correction. The Ratio of minimum to maximum transmission is 0.7119. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.015
_exptl_crystal_description       needle
_exptl_crystal_F_000             1432
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.131
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.023
_refine_diff_density_max         1.183
_refine_diff_density_min         -1.157
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         8254
_refine_ls_number_restraints     180
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0281
_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^)+(0.0180P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0539
_refine_ls_wR_factor_ref         0.0569
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6842
_reflns_number_total             8254
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b09321_si_004.cif
_cod_data_source_block           cx1226a
_cod_original_cell_volume        2443.3(9)
_cod_database_code               4133287
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.858
_shelx_estimated_absorpt_t_min   0.467
_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. Uiso/Uaniso restraints and constraints
C6 \\sim C7 \\sim C8 \\sim C9 \\sim C10: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
C22A \\sim C22 \\sim C21A \\sim C21: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C5 \\sim C5A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C5) \\sim Ueq, Uanis(C5A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 C6, C7, C8, C9, C10
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C22A, C21, C21A, C22
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C2A, C2, C3, C3A, C4, C4A, C5A, C5, C6, C10, C9, C8, C7, C6A, C7A, C8A, C9A,
 C10A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(Cl3A)=Sof(Cl4A)=Sof(C21A)=Sof(H21A)=Sof(H21B)=Sof(C22A)=Sof(H22A)=
 Sof(H22B)=1-FVAR(1)
 Sof(C21)=Sof(H21C)=Sof(H21D)=Sof(C22)=Sof(H22C)=Sof(H22D)=Sof(Cl3)=Sof(Cl4)=
 FVAR(1)
 Sof(Fe1A)=Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=
 Sof(H5A)=Sof(C6A)=Sof(H6A)=Sof(C7A)=Sof(H7A)=Sof(C8A)=Sof(H8A)=Sof(C9A)=
 Sof(H9A)=Sof(C10A)=Sof(H10A)=1-FVAR(2)
 Sof(Fe1)=Sof(C2)=Sof(H2)=Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4)=Sof(C5)=Sof(H5)=
 Sof(C6)=Sof(H6)=Sof(C7)=Sof(H7)=Sof(C8)=Sof(H8)=Sof(C9)=Sof(H9)=Sof(C10)=
 Sof(H10)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C2(H2), C2A(H2A), C3(H3), C3A(H3A), C4(H4), C4A(H4A), C5(H5), C5A(H5A)
5.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C21(H21C,H21D), C21A(H21A,H21B), C22(H22C,
 H22D), C22A(H22A,H22B)
5.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C6A(H6A), C7(H7), C7A(H7A), C8(H8), C8A(H8A), C9(H9), C9A(H9A),
 C10(H10), C10A(H10A), C15(H15), C16(H16), C17(H17), C18(H18)
5.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C)
;
_shelx_res_checksum              53613
_shelx_hkl_checksum              56889
_olex2_date_sample_data_collection 2018-03-06
_olex2_date_sample_submission    2018-03-02
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_olex2_submission_original_sample_id cx1226a
_olex2_submission_special_instructions 'No special instructions were received'