Chiral metal phosphate catalysis: highly asymmetric hetero-Diels-Alder reactions
Tao Liang; Guilong Li; Lukasz Wojtas; Jon C. Antilla; Chem.Commun. 50 (2014) 14187–; doi:10.1039/C4cc06520D

data_7115939
_publ_section_title
;
 Chiral metal phosphate catalysis: highly asymmetric hetero-Diels-Alder
 reactions
;
_journal_name_full               Chem.Commun.
_journal_page_first              14187
_journal_paper_doi               10.1039/C4cc06520D
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C84 H64 Ca O12 P2, C H4 O, C H4 O, H2 O'
_chemical_formula_sum            'C86 H74 Ca O15 P2'
_chemical_formula_weight         1449.47
_chemical_name_systematic
;
 ?
;
_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_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 90.290(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.2594(3)
_cell_length_b                   13.6877(5)
_cell_length_c                   32.5308(11)
_cell_measurement_temperature    100(2)
_cell_volume                     3677.6(2)
_computing_cell_refinement       'APEX2(Bruker,2012);SAINT 8.18C(Bruker,2012)'
_computing_data_collection       'APEX2(Bruker, 2012'
_computing_data_reduction        'SAINT (Bruker,2012);XPREP(Sheldrick,2012)'
_computing_publication_material  'OLEX2 (Dolomanov,2009)'
_computing_structure_refinement  SHELXL-2012Beta(Sheldrick,2012),OLEX2(2009)
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_unetI/netI     0.0981
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            52231
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        66.650
_diffrn_reflns_theta_max         66.500
_diffrn_reflns_theta_min         3.503
_diffrn_source                   'INCOATEC Imus micro-focus source'
_exptl_absorpt_coefficient_mu    1.708
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6376
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; (Sheldrick, 2003)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_description       plate
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.758
_refine_diff_density_min         -0.442
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details
;
 Flack x determined using 4726 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.036(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     962
_refine_ls_number_reflns         52231
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0908
_refine_ls_R_factor_gt           0.0756
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0167P)^2^+13.8003P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1641
_refine_ls_wR_factor_ref         0.1736
_reflns_Friedel_coverage         0.885
_reflns_Friedel_fraction_full    0.949
_reflns_Friedel_fraction_max     0.952
_reflns_number_gt                45390
_reflns_number_total             52231
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc06520d2.cif
_cod_data_source_block           Ca[P4]2
_cod_database_code               7115939
_shelx_estimated_absorpt_t_min   0.848
_shelx_estimated_absorpt_t_max   0.967
_shelxl_version_number           2012-9