CO2-promoted oxidative cross-coupling reaction for C-S bond formation via masked strategy in an odourless way
Zongjun Qiao; Nanyang Ge; Xuefeng Jiang; Chem.Commun. 51 (2015) 10295–; doi:10.1039/C5cc03038B

data_7117309
_publ_section_title
;
 CO2-promoted oxidative cross-coupling reaction for C-S bond formation via
 masked strategy in an odourless way
;
_journal_name_full               Chem.Commun.
_journal_page_first              10295
_journal_paper_doi               10.1039/C5cc03038B
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C8 H24 Cu N4, 2(C7 H6 F O3 S2), 2(H2 O)'
_chemical_formula_sum            'C22 H40 Cu F2 N4 O8 S4'
_chemical_formula_weight         718.36
_chemical_name_systematic
;
 ?
;
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-04-23
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-04-24 deposited with the CCDC.
2015-05-12 downloaded from the CCDC.
;
_cell_angle_alpha                92.852(3)
_cell_angle_beta                 93.152(4)
_cell_angle_gamma                107.116(3)
_cell_formula_units_Z            1
_cell_length_a                   7.5312(15)
_cell_length_b                   8.2038(16)
_cell_length_c                   13.344(3)
_cell_measurement_reflns_used    3444
_cell_measurement_temperature    130
_cell_measurement_theta_max      30.37
_cell_measurement_theta_min      2.60
_cell_volume                     784.9(3)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      130
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0233
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5492
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.996
_diffrn_reflns_theta_min         1.532
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.023
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5134
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0659 before and 0.0349 after correction.
The Ratio of minimum to maximum transmission is 0.6881.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_density_meas      .
_exptl_crystal_description       block
_exptl_crystal_F_000             375
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.860
_refine_diff_density_min         -0.930
_refine_diff_density_rms         0.144
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         3094
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0619
_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^)+(0.0926P)^2^+2.4990P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1716
_refine_ls_wR_factor_ref         0.1777
_reflns_Friedel_coverage         0.000
_reflns_friedel_fraction_full    .
_reflns_friedel_fraction_max     .
_reflns_number_gt                2753
_reflns_number_total             3094
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc03038b2.cif
_cod_data_source_block           mo_dm14546_0m
_cod_database_code               7117309
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.862
_shelx_estimated_absorpt_t_min   0.685
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Free rotating group:
 O4(H4D,H4E)
2.b Ternary CH refined with riding coordinates:
 N1(H1), N2(H2)
2.c Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B)
2.d Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), C9(H9)
2.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C4(H4A,H4B,H4C), C11(H11A,H11B,H11C)
;
_shelx_res_checksum              77793
_shelx_hkl_checksum              23563
_olex2_submission_special_instructions 'No special instructions were received'