Light-initiated reversible conversion of macrocyclic endoperoxides derived from half-sandwich rhodium-based metallarectangles.
Shan, Wei-Long; Gao, Wen-Xi; Lin, Yue-Jian; Jin, Guo-Xin; Dalton transactions (Cambridge, England : 2003) 47 (2018) 2769–2777; doi:10.1039/c7dt03962j

data_7045371
_publ_section_title
;
 Light-initiated reversible conversion of macrocyclic endoperoxides
 derived from half-sandwich rhodium-based metallarectangles.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2769
_journal_page_last               2777
_journal_paper_doi               10.1039/c7dt03962j
_journal_volume                  47
_journal_year                    2018
_chemical_formula_sum            'C108 H118 F12 N4 O25 Rh4 S4'
_chemical_formula_weight         2639.94
_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
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-09-20 deposited with the CCDC.
2018-01-24 downloaded from the CCDC.
;
_cell_angle_alpha                105.9447(19)
_cell_angle_beta                 111.7756(16)
_cell_angle_gamma                94.6228(18)
_cell_formula_units_Z            2
_cell_length_a                   17.0567(6)
_cell_length_b                   17.0598(7)
_cell_length_c                   22.6028(8)
_cell_measurement_reflns_used    9748
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      72.32
_cell_measurement_theta_min      2.81
_cell_volume                     5748.8(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0575
_diffrn_reflns_av_unetI/netI     0.0573
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            66858
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.999
_diffrn_reflns_theta_min         2.229
_exptl_absorpt_coefficient_mu    6.023
_exptl_absorpt_correction_T_max  0.754
_exptl_absorpt_correction_T_min  0.494
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_description       block
_exptl_crystal_F_000             2692
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.180
_platon_squeeze_details
; 
 In asymmetric unit of this data, there were disordered 
 anion and solvents (one triflate anion, three methanol and 
 one water molecules) which could not be restrained 
 properly. Therefore, SQUEEZE algorithm was used to omit 
 them. 
;
_refine_diff_density_max         2.583
_refine_diff_density_min         -1.302
_refine_diff_density_rms         0.144
_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     1421
_refine_ls_number_reflns         20637
_refine_ls_number_restraints     342
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0947
_refine_ls_R_factor_gt           0.0810
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1387P)^2^+22.1454P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2286
_refine_ls_wR_factor_ref         0.2406
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16306
_reflns_number_total             20637
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03962j2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7045371--7045376.cif.'
_cod_database_code               7045371
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.314
_shelx_estimated_absorpt_t_max   0.410
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              96235