Enantioselective catalysts for the Henry reaction: fine-tuning the catalytic components
Constable, Edwin C.; Zhang, Guoqi; Housecroft, Catherine E.; Neuburger, Markus; Schaffner, Silvia; Woggon, Wolf-D.; Zampese, Jennifer A.; New Journal of Chemistry 33 (2009) 2166–; doi:10.1039/b9nj00243j

data_7054133
_publ_section_related_literature
;
?
;
_publ_section_title
;
 Enantioselective catalysts for the Henry reaction: fine-tuning the
 catalytic components
;
_journal_issue                   10
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2166
_journal_paper_doi               10.1039/b9nj00243j
_journal_volume                  33
_journal_year                    2009
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C32 H34 Cu1 N2 O4'
_chemical_formula_sum            'C32 H34 Cu N2 O4'
_chemical_formula_weight         574.18
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             09-05-06
_audit_creation_method           CRYSTALS_ver_12.86
_cell_angle_alpha                90
_cell_angle_beta                 96.926(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.1947(8)
_cell_length_b                   14.0122(8)
_cell_length_c                   9.4085(5)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    123
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     2642.9(2)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      123
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.041
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            76654
_diffrn_reflns_theta_full        34.953
_diffrn_reflns_theta_max         35.666
_diffrn_reflns_theta_min         2.032
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.868
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.96
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1204
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.07
_refine_diff_density_min         -1.10
_refine_ls_abs_structure_details 'Flack (1983), 5786 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.000(5)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0690
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         8030
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0266
_refine_ls_shift/su_max          0.000275
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
0.594 0.213 0.398
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0359
_refine_ls_wR_factor_gt          0.0281
_refine_ls_wR_factor_ref         0.0265
_reflns_limit_h_max              32
_reflns_limit_h_min              -32
_reflns_limit_k_max              22
_reflns_limit_k_min              -22
_reflns_limit_l_max              15
_reflns_limit_l_min              0
_reflns_number_gt                9119
_reflns_number_total             12023
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0240
_oxford_refine_ls_scale          0.24290(16)
_oxford_reflns_number_all        12008
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_oxford_structure_analysis_title 'gq17_123k_0ma in C2'
_cod_data_source_file            b9nj00243j.txt
_cod_data_source_block           gq17_123k
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      'C 2 '
_cod_original_formula_sum        'C32 H34 Cu1 N2 O4'
_cod_database_code               7054133