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_4133286
_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
'C40 H39 Cl Fe N2 P Pt S2, C24 H20 B, C4 H10 O'
_chemical_formula_sum            'C68 H69 B Cl Fe N2 O P Pt S2'
_chemical_formula_weight         1322.54
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-07-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                86.285(3)
_cell_angle_beta                 76.550(3)
_cell_angle_gamma                68.456(3)
_cell_formula_units_Z            2
_cell_length_a                   11.0864(7)
_cell_length_b                   12.6716(8)
_cell_length_c                   23.6012(15)
_cell_measurement_reflns_used    9910
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.480
_cell_measurement_theta_min      2.466
_cell_volume                     2998.6(3)
_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    'ShelXD (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.01
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'QuazarTM optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_unetI/netI     0.0547
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            46366
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.565
_diffrn_reflns_theta_min         1.728
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    2.758
_exptl_absorpt_correction_T_max  0.0998
_exptl_absorpt_correction_T_min  0.0674
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0716 before and 0.0552 after correction. The Ratio of minimum to maximum transmission is 0.9185. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_description       rod
_exptl_crystal_F_000             1344
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.117
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.055
_refine_diff_density_max         5.550
_refine_diff_density_min         -2.380
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     706
_refine_ls_number_reflns         18220
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0525
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0306P)^2^+13.2517P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1172
_refine_ls_wR_factor_ref         0.1203
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16446
_reflns_number_total             18220
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b09321_si_005.cif
_cod_data_source_block           cx1350a
_cod_database_code               4133286
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.863
_shelx_estimated_absorpt_t_min   0.739
_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:
 C11(H11A,H11B), C12(H12A,H12B), C27(H27A,H27B), C28(H28A,H28B), C65(H65A,
 H65B), C67(H67A,H67B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10),
 C15(H15), C16(H16), C17(H17), C18(H18), C22(H22), C23(H23), C24(H24), C25(H25),
  C26(H26), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C36(H36),
 C37(H37), C38(H38), C39(H39), C40(H40), C42(H42), C43(H43), C44(H44), C45(H45),
  C46(H46), C48(H48), C49(H49), C50(H50), C51(H51), C52(H52), C54(H54),
 C55(H55), C56(H56), C57(H57), C58(H58), C60(H60), C61(H61), C62(H62), C63(H63),
  C64(H64)
2.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C66(H66A,H66B,H66C), C68(H68A,H68B,H68C)
;
_shelx_res_checksum              82520
_shelx_hkl_checksum              43555
_olex2_date_sample_data_collection 2018-07-27
_olex2_date_sample_submission    2018-07-18
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in Paratone'
_olex2_submission_original_sample_id cx1350a
_olex2_submission_special_instructions 'No special instructions were received'