Activation of SO<sub>2</sub> by [Zn(Cp*)<sub>2</sub>] and [(Cp*)Zn<sup>I</sup>-Zn<sup>I</sup>(Cp*)].
Kelly, Rory P.; Kazeminejad, Neda; Lamsfus, Carlos A.; Maron, Laurent; Roesky, Peter W.; Chemical communications (Cambridge, England) 52 (2016) 13090–13093; doi:10.1039/c6cc05638e

data_7124927
_publ_section_title
;
 Activation of SO<sub>2</sub> by [Zn(Cp*)<sub>2</sub>] and
 [(Cp*)Zn<sup>I</sup>-Zn<sup>I</sup>(Cp*)].
;
_journal_issue                   89
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              13090
_journal_page_last               13093
_journal_paper_doi               10.1039/c6cc05638e
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C12 H32 N4 O7 S3 Zn2, C4 H8 O'
_chemical_formula_sum            'C16 H40 N4 O8 S3 Zn2'
_chemical_formula_weight         643.44
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-05-26
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-09-01 deposited with the CCDC.
2016-09-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.699(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9030(8)
_cell_length_b                   15.8305(8)
_cell_length_c                   13.4913(9)
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.68
_cell_measurement_theta_min      2.02
_cell_volume                     2677.4(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'STOE StadiVari'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_unetI/netI     0.0725
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12736
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.076
_diffrn_reflns_theta_min         2.017
_exptl_absorpt_coefficient_mu    2.071
_exptl_absorpt_correction_T_max  0.8815
_exptl_absorpt_correction_T_min  0.7516
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED AND X-SHAPE'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.596
_exptl_crystal_description       prism
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.165
_exptl_crystal_size_mid          0.131
_exptl_crystal_size_min          0.069
_refine_diff_density_max         1.337
_refine_diff_density_min         -0.692
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.836
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     351
_refine_ls_number_reflns         5244
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      0.833
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0323
_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^)+(0.0067P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0547
_refine_ls_wR_factor_ref         0.0582
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3763
_reflns_number_total             5244
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc05638e2.cif
_cod_data_source_block           3
_cod_database_code               7124927
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O8A-C13A
 1.45 with sigma of 0.005
 O8A-C13A \\sim O8B-C13B
 with sigma of 0.01
 O8A-C16A \\sim O8B-C16B
 with sigma of 0.02
 C13A-C14A \\sim C13B-C14B
 with sigma of 0.02
 C14A-C15A \\sim C14B-C15B
 with sigma of 0.02
 C15A-C16A \\sim C15B-C16B
 with sigma of 0.02
 O8A-C14A \\sim O8B-C14B
 with sigma of 0.02
 O8A-C15A \\sim O8B-C15B
 with sigma of 0.02
 C13A-C15A \\sim C13B-C15B
 with sigma of 0.02
 C13A-C16A \\sim C13B-C16B
 with sigma of 0.02
 C14A-C16A \\sim C14B-C16B
 with sigma of 0.02
3. Rigid bond restraints
 O8B, C13B, C14B, C15B, C16B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O8B \\sim C13B \\sim C14B \\sim C15B \\sim C16B: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
Uanis(C14B) \\sim Ueq, Uanis(C16B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Others
 Fixed Sof: O8B(0.25) C13B(0.25) H13A(0.25) H13B(0.25) C14B(0.25) H14A(0.25)
 H14B(0.25) C15B(0.25) H15A(0.25) H15B(0.25) C16B(0.25) H16A(0.25) H16B(0.25)
 C15A(0.75) H15C(0.75) H15D(0.75) C13A(0.75) H13C(0.75) H13D(0.75) O8A(0.75)
 C14A(0.75) H14C(0.75) H14D(0.75) C16A(0.75) H16C(0.75) H16D(0.75)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C7(H7A,H7B), C8(H8A,H8B), C13B(H13A,H13B),
 C14B(H14A,H14B), C15B(H15A,H15B), C16B(H16A,H16B), C15A(H15C,H15D), C13A(H13C,
 H13D), C14A(H14C,H14D), C16A(H16C,H16D)
6.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C9(H9A,
 H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              4697
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'