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_7124926
_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         'C60 H90 O13 S6 Zn4, 1.5(C5 H12)'
_chemical_formula_sum            'C67.5 H108 O13 S6 Zn4'
_chemical_formula_weight         1581.37
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-06-01
_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                89.161(4)
_cell_angle_beta                 79.646(4)
_cell_angle_gamma                73.544(4)
_cell_formula_units_Z            2
_cell_length_a                   13.8362(7)
_cell_length_b                   15.0709(8)
_cell_length_c                   20.3113(10)
_cell_measurement_reflns_used    19236
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.89
_cell_measurement_theta_min      1.70
_cell_volume                     3992.8(4)
_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 0.996
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'STOE StadiVari'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1492
_diffrn_reflns_av_unetI/netI     0.1321
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            35842
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.143
_diffrn_reflns_theta_min         1.701
_exptl_absorpt_coefficient_mu    1.397
_exptl_absorpt_correction_T_max  0.9246
_exptl_absorpt_correction_T_min  0.8401
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED & X-SHAPE'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_description       plate
_exptl_crystal_F_000             1666
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.108
_exptl_crystal_size_min          0.058
_refine_diff_density_max         1.571
_refine_diff_density_min         -1.293
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.958
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     956
_refine_ls_number_reflns         15667
_refine_ls_number_restraints     171
_refine_ls_restrained_S_all      0.961
_refine_ls_R_factor_all          0.1389
_refine_ls_R_factor_gt           0.0903
_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^)+(0.1340P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2170
_refine_ls_wR_factor_ref         0.2452
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8729
_reflns_number_total             15667
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc05638e2.cif
_cod_data_source_block           2
_cod_original_formula_sum        'C67.50 H108 O13 S6 Zn4'
_cod_database_code               7124926
_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
 C103-C104
 1.51 with sigma of 0.02
 C52A-C53A \\sim C52B-C53B
 with sigma of 0.01
 C53A-C54A \\sim C53B-C54B
 with sigma of 0.01
 C54A-C55A \\sim C54B-C55B
 with sigma of 0.01
 C55A-C51A \\sim C55B-C51B
 with sigma of 0.01
 C51A-C53A \\sim C51B-C53B
 with sigma of 0.01
 C52A-C54A \\sim C52B-C54B
 with sigma of 0.01
 C53A-C55A \\sim C53B-C55B
 with sigma of 0.01
 C54A-C51A \\sim C54B-C51B
 with sigma of 0.01
 C53A-C58A \\sim C53B-C58B
 with sigma of 0.01
 C52B-C57B \\sim C52A-C57A
 with sigma of 0.01
 C1-S1 \\sim C51A-S6A
 with sigma of 0.01
 C1-S1 \\sim C51B-S6B
 with sigma of 0.01
 S6A-O12A \\sim S6B-O12B
 with sigma of 0.01
 S1-O1 \\sim S6A-O11A
 with sigma of 0.01
 S1-O1 \\sim S6B-O11B
 with sigma of 0.01
 C100-C101 \\sim C105-C106
 with sigma of 0.01
 C101-C102 \\sim C106-C107
 with sigma of 0.01
 C102-C103 \\sim C107-C108
 with sigma of 0.01
 C103-C104 \\sim C108-C109
 with sigma of 0.01
 C101-C103 \\sim C106-C108
 with sigma of 0.04
 C100-C102 \\sim C105-C107
 with sigma of 0.04
 C101-C103 \\sim C106-C108
 with sigma of 0.04
 C102-C104 \\sim C107-C109
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C51A \\sim C51B: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.02
C52A \\sim C52B: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.02
C53A \\sim C53B: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.02
C54A \\sim C54B: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.02
C55A \\sim C55B: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.02
C56A \\sim C56B: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.02
C57A \\sim C57B: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.02
C58A \\sim C58B: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.02
C59A \\sim C59B: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.02
C60A \\sim C60B: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.02
C100 \\sim C101: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.02
C101 \\sim C102: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.02
C102 \\sim C103: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.02
C103 \\sim C104: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.02
C105 \\sim C106: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.02
C106 \\sim C107: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.02
C107 \\sim C108: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.02
C108 \\sim C109: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.02
O11A \\sim O11B: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.02
O12A \\sim O12B: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.02
S6A \\sim S6B: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.02
Uanis(S6A) \\sim Ueq, Uanis(C52B) \\sim Ueq, Uanis(C59B) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: S6A(0.5) O11A(0.5) O12A(0.5) C51A(0.5) C51B(0.5) C52A(0.5)
 C52B(0.5) C53A(0.5) C53B(0.5) C54A(0.5) C54B(0.5) C55A(0.5) C55B(0.5)
 C56A(0.5) H56A(0.5) H56B(0.5) H56C(0.5) C56B(0.5) H56D(0.5) H56E(0.5)
 H56F(0.5) C57A(0.5) H57A(0.5) H57B(0.5) H57C(0.5) C57B(0.5) H57D(0.5)
 H57E(0.5) H57F(0.5) C58A(0.5) H58A(0.5) H58B(0.5) H58C(0.5) C59A(0.5)
 H59A(0.5) H59B(0.5) H59C(0.5) C59B(0.5) H59D(0.5) H59E(0.5) H59F(0.5)
 C60A(0.5) H60A(0.5) H60B(0.5) H60C(0.5) C60B(0.5) H60D(0.5) H60E(0.5)
 H60F(0.5) C58B(0.5) H58D(0.5) H58E(0.5) H58F(0.5) S6B(0.5) O12B(0.5) O11B(0.5)
 C106(0.5) H10P(0.5) H10Q(0.5) C109(0.5) H10R(0.5) H10S(0.5) H10T(0.5)
 C107(0.5) H10U(0.5) H10V(0.5) C105(0.5) H10W(0.5) H10X(0.5) H10Y(0.5)
 C108(0.5) H10Z(0.5) H(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C103(H10G,H10H), C102(H10I,H10J), C101(H10K,H10L), C106(H10P,H10Q), C107(H10U,
 H10V), C108(H10Z,H)
5.b Me refined with riding coordinates:
 C104(H10D,H10E,H10F), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C),
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C),
  C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C26(H26A,H26B,
 H26C), C27(H27A,H27B,H27C), C100(H10M,H10N,H10O), C28(H28A,H28B,H28C),
 C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C36(H36A,H36B,H36C), C37(H37A,H37B,
 H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C46(H46A,
 H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C),
 C50(H50A,H50B,H50C), C56A(H56A,H56B,H56C), C57A(H57A,H57B,H57C), C57B(H57D,
 H57E,H57F), C58A(H58A,H58B,H58C), C59A(H59A,H59B,H59C), C59B(H59D,H59E,H59F),
 C60A(H60A,H60B,H60C), C60B(H60D,H60E,H60F), C58B(H58D,H58E,H58F), C109(H10R,
 H10S,H10T), C105(H10W,H10X,H10Y)
5.c Idealised Me refined as rotating group:
 C56B(H56D,H56E,H56F)
;
_shelx_res_checksum              99728
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'