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_7054135
_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_formula_moiety         'C8 H20 N, Cu2 I3'
_chemical_formula_sum            'C8 H20 Cu2 I3 N'
_chemical_formula_weight         638.06
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             09-05-28
_audit_creation_method           CRYSTALS_ver_12.86
_cell_angle_alpha                90
_cell_angle_beta                 95.4620(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.4552(2)
_cell_length_b                   17.3368(4)
_cell_length_c                   10.8328(2)
_cell_measurement_reflns_used    9457
_cell_measurement_temperature    123
_cell_measurement_theta_max      36
_cell_measurement_theta_min      3
_cell_volume                     1580.73(6)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Bruker Kappa Apex2'
_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  0.032
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            69573
_diffrn_reflns_theta_full        36.386
_diffrn_reflns_theta_max         36.386
_diffrn_reflns_theta_min         2.224
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.521
_exptl_absorpt_correction_T_max  0.84
_exptl_absorpt_correction_T_min  0.18
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 (Bruker AXS, 2006)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.681
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.50
_refine_diff_density_min         -1.55
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0936
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         5956
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0178
_refine_ls_shift/su_max          0.004802
_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:
0.846E-01 0.389E-01 0.295E-01
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0276
_refine_ls_wR_factor_gt          0.0167
_refine_ls_wR_factor_ref         0.0162
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              28
_reflns_limit_k_min              0
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                6302
_reflns_number_total             7681
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.18
_oxford_diffrn_Wilson_scale      314.76
_oxford_refine_ls_r_factor_ref   0.0165
_oxford_refine_ls_scale          0.05828(2)
_oxford_reflns_number_all        7668
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_oxford_structure_analysis_title 'gq71_2_123k_0m in P2(1)/n'
_cod_data_source_file            b9nj00243j.txt
_cod_data_source_block           gq71_2_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.

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' 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      'P 21/n '
_cod_original_formula_sum        'C8 H20 Cu2 I3 N1'
_cod_database_code               7054135