Tuning Rh(II)-catalysed cyclopropanation with tethered thioether ligands.
Cressy, Derek; Zavala, Cristian; Abshire, Anthony; Sheffield, William; Darko, Ampofo; Dalton transactions (Cambridge, England : 2003) 49 (2020) 15779–15787; doi:10.1039/d0dt03019h

data_7706279
_publ_section_title
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 Tuning Rh(II)-catalysed cyclopropanation with tethered thioether ligands.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15779
_journal_page_last               15787
_journal_paper_doi               10.1039/d0dt03019h
_journal_volume                  49
_journal_year                    2020
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C19 H24 N2 O8 Rh2 S'
_chemical_formula_sum            'C19 H24 N2 O8 Rh2 S'
_chemical_formula_weight         646.29
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_Int_Tables_number      4
_atom_sites_solution_primary     dual
_audit_creation_date             2020-04-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-08-04 deposited with the CCDC.	2020-10-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.176(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.9230(9)
_cell_length_b                   28.185(3)
_cell_length_c                   14.6929(13)
_cell_measurement_reflns_used    9654
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.33
_cell_volume                     4523.4(7)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_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  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.9975
_diffrn_measured_fraction_theta_max 0.9975
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0506
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            119747
_diffrn_reflns_theta_full        27.5243
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         2.32
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.600
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6826
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0937 before and 0.0577 after correction.
The Ratio of minimum to maximum transmission is 0.9155.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.8979
_exptl_crystal_description       plate
_exptl_crystal_F_000             2560.2619
_exptl_crystal_recrystallization_method
'Slow evaporation of a mixture of 1:1 MeCN/Toluene'
_exptl_crystal_size_max          0.222
_exptl_crystal_size_mid          0.131
_exptl_crystal_size_min          0.079
_refine_diff_density_max         2.2215
_refine_diff_density_min         -0.6396
_refine_diff_density_rms         0.1067
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   0.032(17)
_refine_ls_d_res_high            0.7690
_refine_ls_d_res_low             8.7789
_refine_ls_goodness_of_fit_ref   1.0607
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    148
_refine_ls_number_parameters     1169
_refine_ls_number_reflns         20769
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.0607
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0280
_refine_ls_shift/su_max          0.0017
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0227P)^2^+8.7717P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0640
_refine_ls_wR_factor_ref         0.0660
_reflns_Friedel_coverage         0.997
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              36
_reflns_limit_k_min              -36
_reflns_limit_l_max              19
_reflns_limit_l_min              -19
_reflns_number_gt                19711
_reflns_number_total             20769
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0dt03019h2.cif
_cod_data_source_block           MonoAspPhTOXTry1full_a
_cod_original_cell_volume        4523.3(7)
_cod_original_sg_symbol_Hall     ' P 2yb'
_cod_database_code               7706279
_olex2_refinement_description
;
;
_olex2_submission_original_sample_id MonoAspPhTOX
_olex2_submission_special_instructions 'No special instructions were received'