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_7045373
_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            'C104 H124 F12 N4 O36 Rh4 S4'
_chemical_formula_weight         2773.94
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                90
_cell_angle_beta                 130.389(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   37.892(4)
_cell_length_b                   16.2390(15)
_cell_length_c                   27.209(5)
_cell_measurement_reflns_used    5663
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      70.34
_cell_measurement_theta_min      3.12
_cell_volume                     12752(3)
_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 0.995
_diffrn_measured_fraction_theta_max 0.978
_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  0.0744
_diffrn_reflns_av_unetI/netI     0.0945
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            33179
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.533
_diffrn_reflns_theta_min         3.122
_exptl_absorpt_coefficient_mu    5.525
_exptl_absorpt_correction_T_max  0.322
_exptl_absorpt_correction_T_min  0.179
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_description       block
_exptl_crystal_F_000             5664
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.090
_platon_squeeze_details
; 
 In asymmetric unit of this data, there were disordered 
 anions and solvents (two triflate anion and six water 
 molecules) which could not be restrained properly. 
 Therefore, SQUEEZE algorithm was used to omit them. 
;
_refine_diff_density_max         2.018
_refine_diff_density_min         -0.544
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     551
_refine_ls_number_reflns         11959
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.1968
_refine_ls_R_factor_gt           0.1175
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3393
_refine_ls_wR_factor_ref         0.3932
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4915
_reflns_number_total             11959
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03962j2.cif
_cod_data_source_block           4-O2
_cod_depositor_comments
'Adding full bibliography for 7045371--7045376.cif.'
_cod_database_code               7045373
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.248
_shelx_estimated_absorpt_t_max   0.636
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              95810