 
data_MR004_a
 
_audit_creation_method            'SHELXL-2016/6'
_shelx_SHELXL_version_number      '2016/6'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'C26 H18 B2 O2, 2(C2 H6 O S)'
_chemical_formula_sum
 'C30 H30 B2 O4 S2' 
_chemical_formula_weight          540.28

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0181   0.0091
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'B'  'B'   0.0090   0.0039
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0492   0.0322
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'S'  'S'   0.3331   0.5567
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       triclinic
_space_group_IT_number            2
_space_group_name_H-M_alt         'P -1'
_space_group_name_Hall            '-P 1'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, -z'
 
_cell_length_a                    5.7757(6)
_cell_length_b                    10.0831(12)
_cell_length_c                    12.4448(14)
_cell_angle_alpha                 70.856(5)
_cell_angle_beta                  84.636(5)
_cell_angle_gamma                 73.657(5)
_cell_volume                      657.00(13)
_cell_formula_units_Z             1
_cell_measurement_temperature     100(2)
_cell_measurement_reflns_used     9918
_cell_measurement_theta_min       3.76
_cell_measurement_theta_max       72.44
 
_exptl_crystal_description        block
_exptl_crystal_colour             yellow
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.366          
_exptl_crystal_F_000              284
_exptl_transmission_factor_min    ?  
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.187
_exptl_crystal_size_mid           0.067
_exptl_crystal_size_min           0.018
_exptl_absorpt_coefficient_mu     2.124
_shelx_estimated_absorpt_T_min    ?
_shelx_estimated_absorpt_T_max    ?
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.6336
_exptl_absorpt_correction_T_max   0.7536
_exptl_absorpt_process_details    Bruker-SADABS
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       100(2)
_diffrn_radiation_wavelength      1.54178
_diffrn_radiation_type            CuK\a
_diffrn_source                    Cu/K(alpha)_ImuS_Microsource               
_diffrn_measurement_device_type   Bruker-Kappa-D8Quest_Photon100 
_diffrn_measurement_method        omega_and_phi_scan
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             13756
_diffrn_reflns_av_unetI/netI      0.0177
_diffrn_reflns_av_R_equivalents   0.0229
_diffrn_reflns_limit_h_min        -7
_diffrn_reflns_limit_h_max        7
_diffrn_reflns_limit_k_min        -12
_diffrn_reflns_limit_k_max        10
_diffrn_reflns_limit_l_min        -15
_diffrn_reflns_limit_l_max        15
_diffrn_reflns_theta_min          3.760
_diffrn_reflns_theta_max          72.424
_diffrn_reflns_theta_full         67.679
_diffrn_measured_fraction_theta_max   0.992
_diffrn_measured_fraction_theta_full  0.995
_diffrn_reflns_Laue_measured_fraction_max    0.992
_diffrn_reflns_Laue_measured_fraction_full   0.995
_diffrn_reflns_point_group_measured_fraction_max   0.992
_diffrn_reflns_point_group_measured_fraction_full  0.995
_reflns_number_total              2582
_reflns_number_gt                 2513
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        'Bruker APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution     'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics     'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details           ?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0489P)²+0.3683P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          2582
_refine_ls_number_parameters      175
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0342
_refine_ls_R_factor_gt            0.0333
_refine_ls_wR_factor_ref          0.0906
_refine_ls_wR_factor_gt           0.0897
_refine_ls_goodness_of_fit_ref    1.057
_refine_ls_restrained_S_all       1.057
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
B1 B -0.1365(3) 0.70795(17) 0.66083(13) 0.0171(3) Uani 1 1 d . . . . .
C1 C 0.0129(3) 0.36294(15) 0.68092(12) 0.0201(3) Uani 1 1 d . . . . .
H1 H -0.127489 0.409823 0.634875 0.024 Uiso 1 1 calc R U . . .
C2 C 0.0661(3) 0.21402(16) 0.73647(13) 0.0216(3) Uani 1 1 d . . . . .
H2 H -0.035337 0.159373 0.726461 0.026 Uiso 1 1 calc R U . . .
C3 C 0.2672(3) 0.14439(15) 0.80671(12) 0.0219(3) Uani 1 1 d . . . . .
H3 H 0.301504 0.042872 0.846173 0.026 Uiso 1 1 calc R U . . .
C4 C 0.4170(3) 0.22465(16) 0.81853(12) 0.0218(3) Uani 1 1 d . . . . .
H4 H 0.554627 0.177778 0.866407 0.026 Uiso 1 1 calc R U . . .
C5 C 0.3674(2) 0.37346(15) 0.76075(12) 0.0193(3) Uani 1 1 d . . . . .
H5 H 0.473289 0.426927 0.768238 0.023 Uiso 1 1 calc R U . . .
C6 C 0.1632(2) 0.44469(14) 0.69189(11) 0.0172(3) Uani 1 1 d . . . . .
C7 C 0.1039(2) 0.60472(14) 0.63423(11) 0.0168(3) Uani 1 1 d . . . . .
C8 C 0.2654(2) 0.66545(14) 0.56529(11) 0.0174(3) Uani 1 1 d . . . . .
H8 H 0.414551 0.602506 0.552639 0.021 Uiso 1 1 calc R U . . .
C9 C 0.2268(2) 0.82159(14) 0.50863(11) 0.0160(3) Uani 1 1 d . . . . .
C10 C 0.4006(2) 0.87127(15) 0.43493(11) 0.0177(3) Uani 1 1 d . . . . .
H10 H 0.541659 0.802976 0.421240 0.021 Uiso 1 1 calc R U . . .
C11 C 0.3729(2) 1.02036(15) 0.37995(11) 0.0177(3) Uani 1 1 d . . . . .
H11 H 0.496283 1.050829 0.330111 0.021 Uiso 1 1 calc R U . . .
C12 C 0.1698(2) 1.12461(15) 0.39651(11) 0.0166(3) Uani 1 1 d . . . . .
C13 C -0.0128(2) 1.07538(14) 0.47158(11) 0.0155(3) Uani 1 1 d . . . . .
C14 C 0.1624(3) 0.61193(17) 1.03560(13) 0.0280(3) Uani 1 1 d . . . . .
H14A H 0.290189 0.520830 1.047232 0.042 Uiso 1 1 calc R U . . .
H14B H 0.008761 0.589862 1.063404 0.042 Uiso 1 1 calc R U . . .
H14C H 0.202005 0.669808 1.077432 0.042 Uiso 1 1 calc R U . . .
C15 C -0.1143(3) 0.85924(16) 0.89684(13) 0.0246(3) Uani 1 1 d . . . . .
H15A H -0.080418 0.900475 0.952940 0.037 Uiso 1 1 calc R U . . .
H15B H -0.257749 0.822969 0.920307 0.037 Uiso 1 1 calc R U . . .
H15C H -0.143165 0.934748 0.822406 0.037 Uiso 1 1 calc R U . . .
O1 O -0.29540(17) 0.64721(10) 0.73358(8) 0.0201(2) Uani 1 1 d . . . . .
H1A H -0.403070 0.712685 0.750824 0.030 Uiso 1 1 calc R U . . .
O2 O 0.35315(19) 0.77458(11) 0.85923(9) 0.0259(2) Uani 1 1 d . . . . .
S1 S 0.13765(6) 0.71267(3) 0.88750(3) 0.01929(12) Uani 1 1 d . . . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
B1 O1 1.3543(18) . ?
B1 C7 1.564(2) . ?
B1 C12 1.565(2) 2_576 ?
C1 C2 1.388(2) . ?
C1 C6 1.397(2) . ?
C1 H1 0.9500 . ?
C2 C3 1.391(2) . ?
C2 H2 0.9500 . ?
C3 C4 1.386(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.393(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.3965(19) . ?
C5 H5 0.9500 . ?
C6 C7 1.4871(18) . ?
C7 C8 1.345(2) . ?
C8 C9 1.4591(18) . ?
C8 H8 0.9500 . ?
C9 C10 1.3817(19) . ?
C9 C13 1.4336(18) 2_576 ?
C10 C11 1.4015(19) . ?
C10 H10 0.9500 . ?
C11 C12 1.3881(19) . ?
C11 H11 0.9500 . ?
C12 C13 1.4276(19) . ?
C13 C13 1.421(3) 2_576 ?
C14 S1 1.7857(16) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 S1 1.7850(15) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
O1 H1A 0.8400 . ?
O2 S1 1.5080(11) . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
O1 B1 C7 118.27(12) . . ?
O1 B1 C12 125.04(12) . 2_576 ?
C7 B1 C12 116.65(12) . 2_576 ?
C2 C1 C6 120.80(13) . . ?
C2 C1 H1 119.6 . . ?
C6 C1 H1 119.6 . . ?
C1 C2 C3 120.32(13) . . ?
C1 C2 H2 119.8 . . ?
C3 C2 H2 119.8 . . ?
C4 C3 C2 119.31(13) . . ?
C4 C3 H3 120.3 . . ?
C2 C3 H3 120.3 . . ?
C3 C4 C5 120.51(13) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 H4 119.7 . . ?
C4 C5 C6 120.50(13) . . ?
C4 C5 H5 119.7 . . ?
C6 C5 H5 119.7 . . ?
C1 C6 C5 118.52(13) . . ?
C1 C6 C7 120.86(12) . . ?
C5 C6 C7 120.59(12) . . ?
C8 C7 C6 120.53(12) . . ?
C8 C7 B1 118.19(12) . . ?
C6 C7 B1 121.04(12) . . ?
C7 C8 C9 124.37(12) . . ?
C7 C8 H8 117.8 . . ?
C9 C8 H8 117.8 . . ?
C10 C9 C13 119.30(12) . 2_576 ?
C10 C9 C8 119.36(12) . . ?
C13 C9 C8 121.34(12) 2_576 . ?
C9 C10 C11 121.34(12) . . ?
C9 C10 H10 119.3 . . ?
C11 C10 H10 119.3 . . ?
C12 C11 C10 121.65(12) . . ?
C12 C11 H11 119.2 . . ?
C10 C11 H11 119.2 . . ?
C11 C12 C13 117.85(12) . . ?
C11 C12 B1 122.95(12) . 2_576 ?
C13 C12 B1 119.18(12) . 2_576 ?
C13 C13 C12 121.22(15) 2_576 . ?
C13 C13 C9 118.63(15) 2_576 2_576 ?
C12 C13 C9 120.15(12) . 2_576 ?
S1 C14 H14A 109.5 . . ?
S1 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
S1 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
S1 C15 H15A 109.5 . . ?
S1 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
S1 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
B1 O1 H1A 109.5 . . ?
O2 S1 C15 106.25(7) . . ?
O2 S1 C14 105.74(7) . . ?
C15 S1 C14 97.47(7) . . ?
 
loop_
 _geom_torsion_atom_site_label_1
 _geom_torsion_atom_site_label_2
 _geom_torsion_atom_site_label_3
 _geom_torsion_atom_site_label_4
 _geom_torsion
 _geom_torsion_site_symmetry_1
 _geom_torsion_site_symmetry_2
 _geom_torsion_site_symmetry_3
 _geom_torsion_site_symmetry_4
 _geom_torsion_publ_flag
C6 C1 C2 C3 1.8(2) . . . . ?
C1 C2 C3 C4 -1.5(2) . . . . ?
C2 C3 C4 C5 0.0(2) . . . . ?
C3 C4 C5 C6 1.3(2) . . . . ?
C2 C1 C6 C5 -0.5(2) . . . . ?
C2 C1 C6 C7 -178.81(12) . . . . ?
C4 C5 C6 C1 -1.1(2) . . . . ?
C4 C5 C6 C7 177.26(12) . . . . ?
C1 C6 C7 C8 -125.77(15) . . . . ?
C5 C6 C7 C8 55.94(19) . . . . ?
C1 C6 C7 B1 60.05(18) . . . . ?
C5 C6 C7 B1 -118.24(14) . . . . ?
O1 B1 C7 C8 -177.59(12) . . . . ?
C12 B1 C7 C8 0.41(18) 2_576 . . . ?
O1 B1 C7 C6 -3.27(19) . . . . ?
C12 B1 C7 C6 174.72(12) 2_576 . . . ?
C6 C7 C8 C9 -177.59(12) . . . . ?
B1 C7 C8 C9 -3.2(2) . . . . ?
C7 C8 C9 C10 -176.68(13) . . . . ?
C7 C8 C9 C13 3.7(2) . . . 2_576 ?
C13 C9 C10 C11 0.6(2) 2_576 . . . ?
C8 C9 C10 C11 -179.01(12) . . . . ?
C9 C10 C11 C12 -0.3(2) . . . . ?
C10 C11 C12 C13 -0.2(2) . . . . ?
C10 C11 C12 B1 178.23(12) . . . 2_576 ?
C11 C12 C13 C13 0.5(2) . . . 2_576 ?
B1 C12 C13 C13 -177.99(14) 2_576 . . 2_576 ?
C11 C12 C13 C9 -179.76(12) . . . 2_576 ?
B1 C12 C13 C9 1.72(19) 2_576 . . 2_576 ?
 
_refine_diff_density_max    0.366
_refine_diff_density_min   -0.320
_refine_diff_density_rms    0.050



