Bis(mandelato)borate: an effective, inexpensive spiroborate anion for chiral resolution
Lawrence W-Y. Wong; Jack W-H. Kan; Thanh-ha Nguyen; Herman H-Y. Sung; Dang Li; Alex S-F. Au-Yeung; Rajpal Sharma; Zhenyang Lin; Ian D. Williams; Chem.Commun. 51 (2015) 15760–; doi:10.1039/C5cc04977F

data_7117979
_publ_section_title
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 Bis(mandelato)borate: an effective, inexpensive spiroborate anion for
 chiral resolution
;
_journal_name_full               Chem.Commun.
_journal_page_first              15760
_journal_paper_doi               10.1039/C5cc04977F
_journal_volume                  51
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C36 H24 Co N6, 3(C16 H12 B O6)'
_chemical_formula_sum            'C84 H60 B3 Co N6 O18'
_chemical_formula_weight         1532.79
_chemical_name_systematic
'Tris-1,10-phenanthroline cobalt(III) Boron(bis-mandelate)'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-10-24
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2014.10.22 svn.r3046 for OlexSys, GUI svn.r4928)
;
_audit_update_record
;
2015-03-02 deposited with the CCDC.
2015-09-02 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   22.7598(4)
_cell_length_b                   74.1769(10)
_cell_length_c                   13.0562(3)
_cell_measurement_temperature    143(2)
_cell_volume                     22042.1(7)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XH (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      143.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_unetI/netI     0.1102
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       96
_diffrn_reflns_limit_k_min       -78
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            69214
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.37
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.317
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             9918
_refine_diff_density_max         0.748
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.047(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2980
_refine_ls_number_reflns         38228
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0912
_refine_ls_R_factor_gt           0.0733
_refine_ls_shift/su_max          10.352
_refine_ls_shift/su_mean         0.202
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0706P)^2^+13.6042P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1552
_refine_ls_wR_factor_ref         0.1643
_reflns_number_gt                30745
_reflns_number_total             38228
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc04977f2.cif
_cod_data_source_block           lawr102m
_cod_database_code               7117979
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C22) \\sim Ueq, Uanis(C163) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.003
3.a Ternary CH refined with riding coordinates:
 C12(H12), C22(H22), C32(H32), C42(H42), C52(H52), C62(H62), C72(H72),
 C82(H82), C92(H92), C102(H102), C112(H112), C122(H122), C132(H132), C142(H142),
  C152(H152), C162(H162), C172(H172), C182(H182)
3.b Aromatic/amide H refined with riding coordinates:
 C201(H201), C202(H202), C203(H203), C206(H206), C207(H207), C210(H210),
 C211(H211), C212(H212), C221(H221), C222(H222), C223(H223), C226(H226),
 C227(H227), C230(H230), C231(H231), C232(H232), C241(H241), C242(H242),
 C243(H243), C246(H246), C247(H247), C250(H250), C251(H251), C252(H252),
 C301(H301), C302(H302), C303(H303), C306(H306), C307(H307), C310(H310),
 C311(H311), C312(H312), C321(H321), C322(H322), C323(H323), C326(H326),
 C327(H327), C330(H330), C331(H331), C332(H332), C341(H341), C342(H342),
 C343(H343), C346(H346), C347(H347), C350(H350), C351(H351), C352(H352),
 C401(H401), C402(H402), C403(H403), C406(H406), C407(H407), C410(H410),
 C411(H411), C412(H412), C421(H421), C422(H422), C423(H423), C426(H426),
 C427(H427), C430(H430), C431(H431), C432(H432), C441(H441), C442(H442),
 C443(H443), C446(H446), C447(H447), C450(H450), C451(H451), C452(H452),
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C24(H24), C25(H25), C26(H26),
  C27(H27), C28(H28), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38),
 C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C54(H54), C55(H55), C56(H56),
  C57(H57), C58(H58), C64(H64), C65(H65), C66(H66), C67(H67), C68(H68),
 C74(H74), C75(H75), C76(H76), C77(H77), C78(H78), C84(H84), C85(H85), C86(H86),
  C87(H87), C88(H88), C94(H94), C95(H95), C96(H96), C97(H97), C98(H98),
 C104(H104), C105(H105), C106(H106), C107(H107), C108(H108), C114(H114),
 C115(H115), C116(H116), C117(H117), C118(H118), C124(H124), C125(H125),
 C126(H126), C127(H127), C128(H128), C134(H134), C135(H135), C136(H136),
 C137(H137), C138(H138), C144(H144), C145(H145), C146(H146), C147(H147),
 C148(H148), C154(H154), C155(H155), C156(H156), C157(H157), C158(H158),
 C164(H164), C165(H165), C166(H166), C167(H167), C168(H168), C174(H174),
 C175(H175), C176(H176), C177(H177), C178(H178), C184(H184), C185(H185),
 C186(H186), C187(H187), C188(H188)
;
_olex2_submission_special_instructions 'No special instructions were received'