Ni(II), Cu(II) and Zn(II) complexes with a sterically hindered scorpionate ligand (Tpms(Ph)) and catalytic application in the diasteroselective nitroaldol (Henry) reaction.
Rocha, Bruno G. M.; Mac Leod, Tatiana C. O.; Guedes da Silva, M Fátima C; Luzyanin, Konstantin V.; Martins, Luísa M D R S; Pombeiro, Armando J. L.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 15192–15200; doi:10.1039/c4dt01509f

data_7032055
_publ_section_title
;
 Ni(II), Cu(II) and Zn(II) complexes with a sterically hindered
 scorpionate ligand (Tpms(Ph)) and catalytic application in the
 diasteroselective nitroaldol (Henry) reaction.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15192
_journal_page_last               15200
_journal_paper_doi               10.1039/c4dt01509f
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C28 H23 Cl Cu N6 O4 S'
_chemical_formula_sum            'C28 H23 Cl Cu N6 O4 S'
_chemical_formula_weight         638.57
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 119.202(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.8172(11)
_cell_length_b                   10.6453(6)
_cell_length_c                   22.5966(14)
_cell_measurement_reflns_used    2807
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.66
_cell_measurement_theta_min      2.29
_cell_volume                     3531.2(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR97 (Giacovazzo et al, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.1248
_diffrn_reflns_av_unetI/netI     0.1463
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            25402
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         2.656
_exptl_absorpt_coefficient_mu    0.790
_exptl_absorpt_correction_T_max  0.9181
_exptl_absorpt_correction_T_min  0.8517
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_description       prism
_exptl_crystal_F_000             1308
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.110
_platon_squeeze_details
;
 The Platon SQUEEZE procedure was applied to recover 333 electrons per
 unit cell (total volume 1002 ^A^3); that is ca. 83 electrons
 per formula unit. Lattice solvent thf molecules (40 electrons/thf)
 were present, and the electrons recovered by SQUEEZE have been assigned
 as 2 thf molecules per formula unit. These thf molecules were not
 included in the formula.
 PLATON Reference : Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13.
;
_refine_diff_density_max         0.910
_refine_diff_density_min         -0.951
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.883
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         6442
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.883
_refine_ls_R_factor_all          0.1202
_refine_ls_R_factor_gt           0.0677
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0884P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1638
_refine_ls_wR_factor_ref         0.1816
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3299
_reflns_number_total             6442
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt01509f2.cif
_cod_data_source_block           Compound4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'MULTI-SCAN' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/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 

 Adding full bibliography for 7032054--7032055.cif.
;
_cod_database_code               7032055
_shelx_estimated_absorpt_t_min   0.852
_shelx_estimated_absorpt_t_max   0.918
_shelxl_version_number           2013-4
_shelx_res_checksum              82873