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_7702052
_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
'3(C72 H96 N8 O8 Se4 Zn), 3(Cl0.33 O1.33), 4(Cl1 O3), 4(O3)'
_chemical_formula_sum            'C216 H288 Cl5 N24 O52 Se12 Zn3'
_chemical_formula_weight         5373.79
_space_group_crystal_system      cubic
_space_group_IT_number           219
_space_group_name_Hall           'F -4a 2 3'
_space_group_name_H-M_alt        'F -4 3 c'
_audit_creation_date             2016-02-24
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  Olex2 1.1
  (compiled Nov  1 2011 20:42:30, GUI svn.r3906)
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2016-02-23 deposited with the CCDC.
2016-02-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
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_cell_length_c                   38.8082(5)
_cell_measurement_reflns_used    3783
_cell_measurement_temperature    150
_cell_measurement_theta_max      70.5900
_cell_measurement_theta_min      4.5300
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
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olex2.refine (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
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_computing_structure_solution
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olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_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 0.9939
_diffrn_measured_fraction_theta_max 0.8351
_diffrn_measurement_details
;
  1 omega  -62.00  -26.00   1.0000    1.5400
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   77.0000   10.0000 36

  2 omega  -17.00   28.00   1.0000    1.5400
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   77.0000   10.0000 45

  3 omega   98.00  167.00   1.0000    1.5400
omega____ theta____ kappa____ phi______ frames
    -      109.9868   77.0000 -169.0000 69

  4 omega  100.00  127.00   1.0000    1.5400
omega____ theta____ kappa____ phi______ frames
    -      109.9868   77.0000  -90.0000 27
;
_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      0.0116971000
_diffrn_orient_matrix_UB_12      -0.0365171000
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_diffrn_orient_matrix_UB_22      0.0053503000
_diffrn_orient_matrix_UB_23      -0.0363508000
_diffrn_orient_matrix_UB_31      0.0348591000
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_diffrn_orient_matrix_UB_33      -0.0122097000
_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  0.0325
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_limit_h_max       31
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_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -45
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_diffrn_reflns_number            10666
_diffrn_reflns_theta_full        71.537939
_diffrn_reflns_theta_max         71.54
_diffrn_reflns_theta_min         4.56
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           n/a
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    2.952
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82504
_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    1.2213
_exptl_crystal_description       block
_exptl_crystal_F_000             21967.2044
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.629106
_refine_diff_density_min         -0.560779
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'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   -0.01(4)
_refine_ls_d_res_high            0.812749
_refine_ls_d_res_low             9.702062
_refine_ls_goodness_of_fit_ref   1.020922
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    37
_refine_ls_number_parameters     240
_refine_ls_number_reflns         4075
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020922
_refine_ls_R_factor_all          0.062882
_refine_ls_R_factor_gt           0.057438
_refine_ls_shift/su_max          4.3678
_refine_ls_shift/su_mean         0.2324
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1339P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.171034
_reflns_Friedel_coverage         0.712
_reflns_limit_h_max              26
_reflns_limit_h_min              -20
_reflns_limit_k_max              46
_reflns_limit_k_min              -45
_reflns_limit_l_max              32
_reflns_limit_l_min              -32
_reflns_number_gt                3709
_reflns_number_total             4075
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c5dt04871k2.cif
_cod_data_source_block           3
_cod_original_cell_volume        58448.3(14)
_cod_original_sg_symbol_Hall     'F -4c 2 3'
_cod_database_code               7702052
_chemical_oxdiff_formula         'C10 H19 N2 O4 Zn'
_reflns_odcompleteness_completeness 99.39
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_submission_special_instructions 'No special instructions were received'