Hydrogen Peroxide Complex of Zinc.
Wallen, Christian M.; Bacsa, John; Scarborough, Christopher C.; Journal of the American Chemical Society 137 (2015) 14606–14609; doi:10.1021/jacs.5b10450

data_4129777
_publ_section_title
;
 Hydrogen Peroxide Complex of Zinc.
;
_journal_issue                   46
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14606
_journal_page_last               14609
_journal_paper_doi               10.1021/jacs.5b10450
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C27 H36 N5 O7 S3 Zn, C16 H36 N'
_chemical_formula_sum            'C43 H72 N6 O7 S3 Zn'
_chemical_formula_weight         946.61
_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             2015-07-13
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2015.06.29 svn.r3191 for OlexSys, GUI svn.r5065)
;
_cell_angle_alpha                90.555(2)
_cell_angle_beta                 100.310(2)
_cell_angle_gamma                110.958(2)
_cell_formula_units_Z            4
_cell_length_a                   13.579(2)
_cell_length_b                   18.615(3)
_cell_length_c                   20.015(4)
_cell_measurement_reflns_used    9762
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.742
_cell_measurement_theta_min      2.384
_cell_volume                     4633.3(14)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2011.2-4 (Bruker, 2011)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'Superflip (L. Palatinus & G. Chapuis, 2007)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans with a narrow frame width'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            77125
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         1.504
_diffrn_source                   'sealed tube'
_diffrn_source_current           35
_diffrn_source_voltage           45
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.720
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6355
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1626 before and 0.0570 after correction.
The Ratio of minimum to maximum transmission is 0.8518.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_description       prism
_exptl_crystal_F_000             2024
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of THF and diethyl ether by vapor diffusion'
_exptl_crystal_size_max          0.627
_exptl_crystal_size_mid          0.279
_exptl_crystal_size_min          0.205
_refine_diff_density_max         1.174
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1335
_refine_ls_number_reflns         21226
_refine_ls_number_restraints     606
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0795
_refine_ls_R_factor_gt           0.0541
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0415P)^2^+12.1864P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1162
_refine_ls_wR_factor_ref         0.1356
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16159
_reflns_number_total             21226
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b10450_si_002.cif
_cod_data_source_block           cmw04_butsnh2oh
_cod_original_cell_volume        4633.2(14)
_cod_database_code               4129777
_shelx_estimated_absorpt_t_max   0.866
_shelx_estimated_absorpt_t_min   0.661
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C26A-C25A
 1.52 with sigma of 0.02
 C28B-C27B
 1.52 with sigma of 0.01
 C29A-C30A = C29B-C30B
 1.52 with sigma of 0.01
 C24B-C23B
 1.52 with sigma of 0.01
 C29A-C30A = C29B-C30B
 1.52 with sigma of 0.004
 S3BB-N2BB \\sim S3BA-N2BA
 with sigma of 0.003
 S3BA-C14_3 \\sim S3BB-C14_4
 with sigma of 0.003
 C17_6-C16_6 \\sim C16_6-C15_6 \\sim C20_6-C19_6 \\sim C19_6-C17_6
 with sigma of 0.02
 C17_6-C20_6 \\sim C17_6-C15_6 \\sim C16_6-C19_6 \\sim C15_6-C20_6
 with sigma of 0.04
3. Restrained planarity
 C17_6, C16_6, C15_6, C20_6, C19_6
 with sigma of 0.1
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C17_6 \\sim C16_6 \\sim C15_6 \\sim C20_6 \\sim C19_6: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C33A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(N7A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C29A) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C31B) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C36A) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C35B) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C33A) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C34A) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C25B) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C25A) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C21A) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(C22A) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C23A) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C33A) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(O5BA) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C14_2) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of
0.004
Uanis(C14_3) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of
0.004
Uanis(C19_4) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of
0.004
Uanis(N2BA) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(O5BA) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(S3BB) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(O6BB) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C34B) = Uanis(C34A)
Uanis(C29A) = Uanis(C29B)
Uanis(C30A) = Uanis(C30B)
Uanis(C33A) = Uanis(C33B)
Uanis(C35A) = Uanis(C35B)
Uanis(O5BA) = Uanis(O5BB)
Uanis(N2BA) = Uanis(N2BB)
Uanis(O6BB) = Uanis(O6BA)
Uanis(C15_2) = Uanis(C15_1)
Uanis(C15_3) = Uanis(C15_4)
Uanis(C14_1) = Uanis(C14_2)
Uanis(C14_4) = Uanis(C14_3)
Uanis(C19_3) = Uanis(C19_4)
Uanis(S3BB) = Uanis(S3BA)
5. Rigid body (RIGU) restrains
 C21B, C22B, C23B, C24B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C25B, C26B, C27B, C28B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N1B, N2BB, C2B, C1B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 N1B, N3B, N4B, C3B, C4B, C5B, C6B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C17_1, C16_1, C15_1, C20_1, C18_1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C17_6, C16_6, C15_6, C20_6, C19_6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C29A, C30A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C31B, C30A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C14_3, C15_3, C16_4, C17_4, C18_4, C19_4, C20_4, C14_4
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C15_2, C16_2, C17_2, C19_2, C20_2, C14_2
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Same fragment restrains
{N7B, C21B, C22B, C23B, C24B, C25B, C26B, C27B, C28B, C29B, C30B, C31B, C32B,
C33B, C34B, C35B, C36B} sigma for 1-2: 0.002, 1-3: 0.002
as
{N7A, C21A, C22A, C23A, C24A, C25A, C26A, C27A, C28A, C29A, C30A, C31A, C32A,
C33A, C34A, C35A, C36A}
{C14_2, C15_2, C16_2, C17_2, C18_2, C19_2, C20_2}
{C14_3, C15_3, C16_3, C17_3, C18_3, C19_3, C20_3}
{C14_4, C15_4, C16_4, C17_4, C18_4, C19_4, C20_4}
{C14_5, C15_5, C16_5, C17_5, C18_5, C19_5, C20_5}
{C14_6, C15_6, C16_6, C17_6, C18_6, C19_6, C20_6}
as
{C14_1, C15_1, C16_1, C17_1, C18_1, C19_1, C20_1} sigma for 1-2: 0.002 1-3:
0.002
7. Others
 Sof(N7B)=Sof(C21B)=Sof(H21C)=Sof(H21D)=Sof(C22B)=Sof(H22C)=Sof(H22D)=
 Sof(C23B)=Sof(H23C)=Sof(H23D)=Sof(C24B)=Sof(H24D)=Sof(H24E)=Sof(H24F)=
 Sof(C25B)=Sof(H25C)=Sof(H25D)=Sof(C26B)=Sof(H26C)=Sof(H26D)=Sof(C27B)=
 Sof(H27C)=Sof(H27D)=Sof(C28B)=Sof(H28F)=Sof(H28G)=Sof(H28H)=Sof(C29B)=
 Sof(H29E)=Sof(H29F)=Sof(C30B)=Sof(H30E)=Sof(H30F)=Sof(C31B)=Sof(H31F)=
 Sof(H31G)=Sof(C32B)=Sof(H32F)=Sof(H32G)=Sof(H32H)=Sof(C33B)=Sof(H33E)=
 Sof(H33F)=Sof(C34B)=Sof(H34E)=Sof(H34F)=Sof(C35B)=Sof(H35F)=Sof(H35G)=
 Sof(C36B)=Sof(H36F)=Sof(H36G)=Sof(H36H)=1-FVAR(1)
 Sof(N7A)=Sof(C21A)=Sof(H21A)=Sof(H21B)=Sof(C22A)=Sof(H22A)=Sof(H22B)=
 Sof(C23A)=Sof(H23A)=Sof(H23B)=Sof(C24A)=Sof(H24A)=Sof(H24B)=Sof(H24C)=
 Sof(C25A)=Sof(H25A)=Sof(H25B)=Sof(C26A)=Sof(H26A)=Sof(H26B)=Sof(C27A)=
 Sof(H27A)=Sof(H27B)=Sof(C28A)=Sof(H28C)=Sof(H28D)=Sof(H28E)=Sof(C29A)=
 Sof(H29C)=Sof(H29D)=Sof(C30A)=Sof(H30C)=Sof(H30D)=Sof(C31A)=Sof(H31D)=
 Sof(H31E)=Sof(C32A)=Sof(H32C)=Sof(H32D)=Sof(H32E)=Sof(C33A)=Sof(H33C)=
 Sof(H33D)=Sof(C34A)=Sof(H34C)=Sof(H34D)=Sof(C35A)=Sof(H35D)=Sof(H35E)=
 Sof(C36A)=Sof(H36C)=Sof(H36D)=Sof(H36E)=FVAR(1)
 Fixed Sof: S3BA(0.5) S3BB(0.5) O5BA(0.5) O5BB(0.5) O6BA(0.5) O6BB(0.5)
 N2BA(0.5) N2BB(0.5) H2BA(0.5) H2BB(0.5) H2BC(0.5) H2BD(0.5) C14(0.5) C15(0.5)
 H15(0.5) C16(0.5) H16(0.5) C17(0.5) C18(0.5) H18A(0.5) H18B(0.5) H18C(0.5)
 C19(0.5) H19(0.5) C20(0.5) H20(0.5) C14(0.5) C15(0.5) H15(0.5) C16(0.5)
 H16(0.5) C17(0.5) C18(0.5) H18A(0.5) H18B(0.5) H18C(0.5) C19(0.5) H19(0.5)
 C20(0.5) H20(0.5) C14(0.5) C15(0.5) H15(0.5) C16(0.5) H16(0.5) C17(0.5)
 C18(0.5) H18A(0.5) H18B(0.5) H18C(0.5) C19(0.5) H19(0.5) C20(0.5) H20(0.5)
 C14(0.5) C15(0.5) H15(0.5) C16(0.5) H16(0.5) C17(0.5) C18(0.5) H18A(0.5)
 H18B(0.5) H18C(0.5) C19(0.5) H19(0.5) C20(0.5) H20(0.5)
8.a Secondary CH2 refined with riding coordinates:
 N5(H5A,H5B), C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C6(H6A,H6B),
 C5(H5C,H5D), N5B(H5BA,H5BB), C2B(H2BA,H2BB), C2B(H2BC,H2BD), C3B(H3BA,H3BB),
 C4B(H4BA,H4BB), C5B(H5BC,H5BD), C1B(H1BA,H1BB), C6B(H6BA,H6BB), C28(H28A,H28B),
  C29(H29A,H29B), C30(H30A,H30B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,
 H34B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C40(H40A,H40B),
 C41(H41A,H41B), C42(H42A,H42B), C21A(H21A,H21B), C22A(H22A,H22B), C23A(H23A,
 H23B), C25A(H25A,H25B), C26A(H26A,H26B), C27A(H27A,H27B), C29A(H29C,H29D),
 C30A(H30C,H30D), C31A(H31D,H31E), C33A(H33C,H33D), C34A(H34C,H34D), C35A(H35D,
 H35E), C21B(H21C,H21D), C22B(H22C,H22D), C23B(H23C,H23D), C25B(H25C,H25D),
 C26B(H26C,H26D), C27B(H27C,H27D), C29B(H29E,H29F), C30B(H30E,H30F), C31B(H31F,
 H31G), C33B(H33E,H33F), C34B(H34E,H34F), C35B(H35F,H35G)
8.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C12(H12), C11(H11), C9(H9), C8B(H8B), C9B(H9B), C11B(H11B),
 C12B(H12B), C15(H15), C16(H16), C19(H19), C20(H20), C15(H15), C16(H16),
 C19(H19), C20(H20), C15(H15), C16(H16), C19(H19), C20(H20), C15(H15), C16(H16),
  C19(H19), C20(H20), C15(H15), C16(H16), C19(H19), C20(H20), C15(H15),
 C16(H16), C19(H19), C20(H20)
8.c Idealised Me refined as rotating group:
 C13(H13D,H13E,H13F), C13B(H13A,H13B,H13C), C31(H31A,H31B,H31C), C35(H35A,H35B,
 H35C), C39(H39A,H39B,H39C), C43(H43A,H43B,H43C), C24A(H24A,H24B,H24C),
 C28A(H28C,H28D,H28E), C32A(H32C,H32D,H32E), C36A(H36C,H36D,H36E), C24B(H24D,
 H24E,H24F), C28B(H28F,H28G,H28H), C32B(H32F,H32G,H32H), C36B(H36F,H36G,H36H),
 C18(H18A,H18B,H18C), C18(H18A,H18B,H18C), C18(H18A,H18B,H18C), C18(H18A,H18B,
 H18C), C18(H18A,H18B,H18C), C18(H18A,H18B,H18C)
8.d Idealised tetrahedral OH refined as rotating group:
 O7(H7), O7B(H7B)
;
_shelx_res_checksum              98709
_shelx_hkl_checksum              2934
_shelx_shelxl_version_number     2014/7
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a loop with paratone oil'
_olex2_submission_original_sample_id CMW04_BuTsNH2OH
_olex2_submission_special_instructions 'No special instructions were received'