Six States Switching of Redox-Active Molecular Tweezers by Three Orthogonal Stimuli.
Doistau, Benjamin; Benda, Lorien; Cantin, Jean-Louis; Chamoreau, Lise-Marie; Ruiz, Eliseo; Marvaud, Valérie; Hasenknopf, Bernold; Vives, Guillaume; Journal of the American Chemical Society 139 (2017) 9213–9220; doi:10.1021/jacs.7b02945

data_4131284
_publ_section_title
;
 Six States Switching of Redox-Active Molecular Tweezers by Three
 Orthogonal Stimuli.
;
_journal_issue                   27
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9213
_journal_page_last               9220
_journal_paper_doi               10.1021/jacs.7b02945
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         'C53 H54 Br N5 Ni O2, C H2 Cl2'
_chemical_formula_sum            'C54 H56 Br Cl2 N5 Ni O2'
_chemical_formula_weight         1016.55
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   41.7129(8)
_cell_length_b                   7.09050(10)
_cell_length_c                   17.3156(3)
_cell_measurement_reflns_used    8660
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      67.28
_cell_measurement_theta_min      3.32
_cell_volume                     5121.35(15)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SUPERFLIP
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multi layer miror'
_diffrn_radiation_source         'micro focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54183
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            6416
_diffrn_reflns_point_group_measured_fraction_full 0.701
_diffrn_reflns_point_group_measured_fraction_max 0.701
_diffrn_reflns_theta_full        66.999
_diffrn_reflns_theta_max         66.999
_diffrn_reflns_theta_min         3.317
_exptl_absorpt_coefficient_mu    2.765
_exptl_absorpt_correction_T_max  0.753
_exptl_absorpt_correction_T_min  0.577
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS, Bruker AXS Inc., Madison, 
Wisconsin, USA. 
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.878
_refine_diff_density_min         -0.684
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details
;
 Flack x determined using 1503 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.103(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     571
_refine_ls_number_reflns         6416
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0491
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0772P)^2^+3.5679P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1350
_refine_ls_wR_factor_ref         0.1373
_reflns_Friedel_coverage         0.380
_reflns_Friedel_fraction_full    0.401
_reflns_Friedel_fraction_max     0.400
_reflns_number_gt                6024
_reflns_number_total             6416
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b02945_si_003.cif
_cod_data_source_block           shelx
_cod_database_code               4131284
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              50795
_shelx_hkl_checksum              33054
_shelx_fab_checksum              20868