Countercation-directed chiral resolution of [Mo2O4(H2dtpa)]−, syntheses, crystal structures and CD spectra of (λ)-[NEt4][Mo2O4(H2dtpa)] and (δ)-Na[Mo2O4(H2dtpa)]
Li, Fengcai; Xu, Li; CrystEngComm 14 (2012) 5174–; doi:10.1039/c2ce25874a

data_7208406
_publ_section_title
;
 Countercation-directed chiral resolution of [Mo2O4(H2dtpa)]&#x2212;,
 syntheses, crystal structures and CD spectra of
 (\l)-[NEt4][Mo2O4(H2dtpa)] and (\d)-Na[Mo2O4(H2dtpa)]
;
_journal_issue                   16
_journal_name_full               CrystEngComm
_journal_page_first              5174
_journal_paper_doi               10.1039/c2ce25874a
_journal_volume                  14
_journal_year                    2012
_chemical_absolute_configuration unk
_chemical_formula_sum            'C14 H26 Mo2 N3 Na O17'
_chemical_formula_weight         723.25
_chemical_name_systematic
;
?
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                71.991(12)
_cell_angle_beta                 76.257(15)
_cell_angle_gamma                83.426(14)
_cell_formula_units_Z            1
_cell_length_a                   7.529(3)
_cell_length_b                   7.752(3)
_cell_length_c                   10.903(3)
_cell_measurement_reflns_used    2109
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4816
_cell_measurement_theta_min      2.7657
_cell_volume                     587.3(4)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  Mercury
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0174
_diffrn_reflns_av_sigmaI/netI    0.0513
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5042
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    1.176
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7159
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    2.045
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Chip
_exptl_crystal_F_000             362
_exptl_crystal_size_max          0.3990
_exptl_crystal_size_mid          0.2010
_exptl_crystal_size_min          0.0950
_refine_diff_density_max         0.427
_refine_diff_density_min         -0.984
_refine_diff_density_rms         0.168
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         3599
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0223
_refine_ls_R_factor_gt           0.0206
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0353P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0504
_refine_ls_wR_factor_ref         0.0720
_reflns_number_gt                3359
_reflns_number_total             3599
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce25874a.txt
_cod_data_source_block           (A)-2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        587.2(4)
_cod_original_sg_symbol_Hall     P1
_cod_original_sg_symbol_H-M      P1
_cod_database_code               7208406