Facile access to zinc and cadmium selones: highly active catalysts for Barbier reactions in aqueous media.
Naga Babu, Chatla; Srinivas, Katam; Prabusankar, Ganesan; Dalton transactions (Cambridge, England : 2003) 45 (2016) 6456–6465; doi:10.1039/c5dt04871k

data_7702055
_publ_section_title
;
 Facile access to zinc and cadmium selones: highly active catalysts for
 Barbier reactions in aqueous media.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6456
_journal_page_last               6465
_journal_paper_doi               10.1039/c5dt04871k
_journal_volume                  45
_journal_year                    2016
_chemical_absolute_configuration unk
_chemical_formula_moiety
'C30 H36 N4 O4 Se2 Zn, 2(Cl O4), 2(H2 O), 0.5(H2 O2)'
_chemical_formula_sum            'C30 H41 Cl2 N4 O15 Se2 Zn'
_chemical_formula_weight         991.90
_space_group_crystal_system      tetragonal
_space_group_IT_number           95
_space_group_name_Hall           'P 4cw 2c'
_space_group_name_H-M_alt        'P 43 2 2'
_symmetry_Int_Tables_number      95
_audit_creation_date             2016-02-13
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-02-13 deposited with the CCDC.
2016-02-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.82385(11)
_cell_length_b                   11.82385(11)
_cell_length_c                   28.5490(4)
_cell_measurement_reflns_used    6033
_cell_measurement_temperature    150
_cell_measurement_theta_max      70.7540
_cell_measurement_theta_min      4.0460
_cell_volume                     3991.25(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1293
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9771
_diffrn_measured_fraction_theta_max 0.9771
_diffrn_measurement_details
;
  1 omega   -7.00   20.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -150.0000 27

  2 omega   31.00   58.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -150.0000 27

  3 omega  -78.00  -52.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000 -156.0000  137.0000 26

  4 omega  -78.00  -34.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  178.0000 -180.0000 44

  5 omega  -33.00   16.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   38.0000 -150.0000 49

  6 omega -119.00  -81.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  178.0000 -180.0000 38

  7 omega -112.00  -85.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000 -156.0000 -174.0000 27

  8 omega   38.00   69.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      109.7185  -38.0000    0.0000 31

  9 omega   53.00   95.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      109.7185  -63.0000   30.0000 42

 10 omega   90.00  170.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      109.7185   38.0000  -60.0000 80

 11 omega   85.00  178.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      109.7185   38.0000   30.0000 93

 12 omega  -69.00   21.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000   60.0000 90

 13 omega   11.00  128.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       54.8593   19.0000 -120.0000 117
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0454556000
_diffrn_orient_matrix_UB_12      0.0297015000
_diffrn_orient_matrix_UB_13      -0.0490509000
_diffrn_orient_matrix_UB_21      0.0735418000
_diffrn_orient_matrix_UB_22      0.0942635000
_diffrn_orient_matrix_UB_23      0.0214761000
_diffrn_orient_matrix_UB_31      0.0974646000
_diffrn_orient_matrix_UB_32      -0.0849134000
_diffrn_orient_matrix_UB_33      0.0066911000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            10355
_diffrn_reflns_theta_full        71.2362
_diffrn_reflns_theta_max         71.24
_diffrn_reflns_theta_min         3.74
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.785
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53892
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.6506
_exptl_crystal_description       block
_exptl_crystal_F_000             2000.0960
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.1957
_refine_diff_density_min         -1.1758
_refine_diff_density_rms         0.1552
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   0.07(5)
_refine_ls_d_res_high            0.8142
_refine_ls_d_res_low             11.8238
_refine_ls_goodness_of_fit_ref   1.0404
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    32
_refine_ls_number_parameters     255
_refine_ls_number_reflns         3794
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0404
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0619
_refine_ls_shift/su_max          2.1260
_refine_ls_shift/su_mean         0.1479
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1344P)^2^+3.2042P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1744
_refine_ls_wR_factor_ref         0.1838
_reflns_Friedel_coverage         0.950
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              10
_reflns_limit_k_min              -9
_reflns_limit_l_max              34
_reflns_limit_l_min              -34
_reflns_number_gt                3525
_reflns_number_total             3794
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c5dt04871k2.cif
_cod_data_source_block           6
_cod_original_cell_volume        3991.24(8)
_cod_original_sg_symbol_Hall     ' P 4cw 2c'
_cod_database_code               7702055
_chemical_oxdiff_formula         'C10 H19 N2 O4 Se Zn'
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Others
 Fixed Sof: H7(0.5)
3.a Free rotating group:
 O6(H6d,H6e), O7(H7)
3.b Secondary CH2 refined with riding coordinates:
 C4(H4a,H4b)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C11(H11), C2(H2), C9(H9)
3.d Idealised Me refined as rotating group:
 C14(H14a,H14b,H14c), C15(H15a,H15b,H15c), C13(H13a,H13b,H13c), C6(H6a,H6b,H6c)
;
_olex2_submission_special_instructions 'No special instructions were received'