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_7702050
_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_formula_moiety         'C36 H48 Cd Cl N5 O7 Se2'
_chemical_formula_sum            'C36 H48 Cd Cl N5 O7 Se2'
_chemical_formula_weight         968.59
_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_Int_Tables_number      14
_audit_creation_date             2016-02-01
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Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
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_audit_update_record
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2016-02-01 deposited with the CCDC.
2016-02-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.816(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_length_c                   26.6168(9)
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_cell_measurement_temperature    150
_cell_measurement_theta_max      71.2190
_cell_measurement_theta_min      4.3170
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_computing_cell_refinement
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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_collection
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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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_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    'Olex2 (Dolomanov et al., 2009)'
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_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 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 0.9787
_diffrn_measured_fraction_theta_max 0.9771
_diffrn_measurement_details
;
  1 omega   29.00   69.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000    0.0000 40

  2 omega  -16.00   10.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000    0.0000 26

  3 omega  -57.00  -29.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -77.0000  -90.0000 28

  4 omega -113.00  -12.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000  150.0000 101

  5 omega  -31.00   30.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   38.0000   90.0000 61

  6 omega  -51.00   -7.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   25.0000  -60.0000 44

  7 omega  -16.00   25.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   38.0000  -60.0000 41

  8 omega  -72.00  -35.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -57.0000    0.0000 37

  9 omega   41.00   93.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      109.7185  -25.0000   90.0000 52

 10 omega   38.00   70.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      109.7185  -38.0000  -30.0000 32

 11 omega   38.00   89.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      109.7185  -25.0000  150.0000 51

 12 omega   89.00  151.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      109.7185  178.0000   60.0000 62

 13 omega   40.00  102.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      109.7185  -50.0000   30.0000 62

 14 omega   44.00  132.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      109.7185  -63.0000 -180.0000 88

 15 omega   41.00   67.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      109.7185  -25.0000 -120.0000 26

 16 omega  104.00  160.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      109.7185  111.0000 -180.0000 56

 17 omega   87.00  169.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      109.7185   25.0000    0.0000 82
;
_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      -0.0794770000
_diffrn_orient_matrix_UB_12      -0.0583276000
_diffrn_orient_matrix_UB_13      0.0260247000
_diffrn_orient_matrix_UB_21      -0.0267503000
_diffrn_orient_matrix_UB_22      -0.0754860000
_diffrn_orient_matrix_UB_23      -0.0487263000
_diffrn_orient_matrix_UB_31      0.0541300000
_diffrn_orient_matrix_UB_32      -0.1217075000
_diffrn_orient_matrix_UB_33      0.0176720000
_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  0.0428
_diffrn_reflns_av_unetI/netI     0.0546
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            14393
_diffrn_reflns_theta_full        71.1129
_diffrn_reflns_theta_max         71.11
_diffrn_reflns_theta_min         3.32
_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    7.341
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.20127
_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    1.5742
_exptl_crystal_description       block
_exptl_crystal_F_000             1952.5686
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.2696
_refine_diff_density_min         -2.3233
_refine_diff_density_rms         0.1746
_refine_ls_d_res_high            0.8148
_refine_ls_d_res_low             13.3017
_refine_ls_goodness_of_fit_ref   1.0375
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    74
_refine_ls_number_parameters     478
_refine_ls_number_reflns         7737
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0375
_refine_ls_R_factor_all          0.0760
_refine_ls_R_factor_gt           0.0690
_refine_ls_shift/su_max          0.0382
_refine_ls_shift/su_mean         0.0039
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1368P)^2^+0.8036P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1884
_refine_ls_wR_factor_ref         0.2036
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              18
_reflns_limit_h_min              -18
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_reflns_limit_k_min              0
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_reflns_limit_l_min              0
_reflns_number_gt                6544
_reflns_number_total             7737
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c5dt04871k2.cif
_cod_data_source_block           1
_cod_original_cell_volume        4086.7(3)
_cod_database_code               7702050
_chemical_oxdiff_formula         'C10 H19 N2 O4 Se Cd'
_reflns_odcompleteness_completeness 99.95
_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
2.a Ternary CH refined with riding coordinates:
 C13(H13), C16(H16), C32(H32), C34(H34)
2.b Secondary CH2 refined with riding coordinates:
 C4(H4a,H4b), C22(H22a,H22b)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C9(H9), C10(H10), C11(H11), C20(H20), C21(H21), C27(H27),
 C28(H28), C29(H29)
2.d Idealised Me refined as rotating group:
 C6(H6a,H6b,H6c), C14(H14a,H14b,H14c), C15(H15a,H15b,H15c), C17(H17a,H17b,
 H17c), C18(H18a,H18b,H18c), C24(H24a,H24b,H24c), C31(H31a,H31b,H31c), C33(H33a,
 H33b,H33c), C35(H35a,H35b,H35c), C36(H36a,H36b,H36c)
;
_olex2_submission_special_instructions 'No special instructions were received'