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_4129775
_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 H35 N4 O7 S3 Zn, C16 H36 N'
_chemical_formula_sum            'C43 H71 N5 O7 S3 Zn'
_chemical_formula_weight         931.59
_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   mixed
_audit_creation_date             2015-05-21
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2015.05.19 svn.r3182 for OlexSys, GUI svn.r5037)
;
_cell_angle_alpha                98.2422(18)
_cell_angle_beta                 92.1817(19)
_cell_angle_gamma                108.3957(18)
_cell_formula_units_Z            4
_cell_length_a                   13.4908(18)
_cell_length_b                   18.694(3)
_cell_length_c                   19.366(3)
_cell_measurement_reflns_used    9792
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.41
_cell_measurement_theta_min      2.36
_cell_volume                     4568.5(12)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2014.1-1 (Bruker, 2014)'
_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 1.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \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  0.0364
_diffrn_reflns_av_unetI/netI     0.0398
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_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            73265
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.435
_diffrn_reflns_theta_min         1.597
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           30
_diffrn_source_voltage           45
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.728
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6225
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1135 before and 0.0459 after correction.
The Ratio of minimum to maximum transmission is 0.8348.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_description       prism
_exptl_crystal_F_000             1992
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of DCM and diethyl ether by vapor diffusion'
_exptl_crystal_size_max          0.587
_exptl_crystal_size_mid          0.423
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.299
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1079
_refine_ls_number_reflns         22779
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0431
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0644P)^2^+1.8894P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1087
_refine_ls_wR_factor_ref         0.1204
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17786
_reflns_number_total             22779
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b10450_si_002.cif
_cod_data_source_block           cmw04_057buzntsaq
_cod_original_cell_volume        4568.7(11)
_cod_database_code               4129775
_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, All O(H,H) groups
2.a Rotating group:
 O1W(H1WA,H1WB), O1WB(H1WC,H1WD)
2.b Secondary CH2 refined with riding coordinates:
 C68(H68A,H68B), C73(H73A,H73B), C65(H65A,H65B), C72(H72A,H72B), C3B(H3BA,
 H3BB), C75(H75A,H75B), C64(H64A,H64B), C84(H84A,H84B), C61(H61A,H61B), C3(H3A,
 H3B), C57(H57A,H57B), C1(H1A,H1B), C85(H85A,H85B), C4(H4A,H4B), C4B(H4BA,H4BB),
  C56(H56A,H56B), C5B(H5BA,H5BB), C5(H5A,H5B), C80(H80A,H80B), C67(H67A,H67B),
 C77(H77A,H77B), C69(H69A,H69B), C6B(H6BA,H6BB), C55(H55A,H55B), C1B(H1BA,H1BB),
  C63(H63A,H63B), C79(H79A,H79B), C59(H59A,H59B), C71(H71A,H71B), C81(H81A,
 H81B), C83(H83A,H83B), C6(H6A,H6B), C2(H2A,H2B), C60(H60A,H60B), C2B(H2BA,
 H2BB), C76(H76A,H76B)
2.c Aromatic/amide H refined with riding coordinates:
 C23(H23), C18(H18), C25(H25), C8B(H8B), C23B(H23B), C9B(H9B), C19(H19),
 C8(H8), C11B(H11B), C9(H9), C11(H11), C22B(H22B), C19B(H19B), C12(H12),
 C26(H26), C22(H22), C18B(H18B), C16(H16), C15(H15), C25B(H25B), C15B(H15B),
 C12B(H12B), C16B(H16B), C26B(H26B)
2.d Idealised Me refined as rotating group:
 C20B(H20D,H20E,H20F), C78(H78A,H78B,H78C), C20(H20A,H20B,H20C), C66(H66A,H66B,
 H66C), C13B(H13D,H13E,H13F), C70(H70A,H70B,H70C), C13(H13A,H13B,H13C),
 C27(H27A,H27B,H27C), C82(H82A,H82B,H82C), C74(H74A,H74B,H74C), C62(H62A,H62B,
 H62C), C27B(H27D,H27E,H27F), C58(H58A,H58B,H58C), C86(H86A,H86B,H86C)
;
_shelx_res_checksum              43041
_shelx_hkl_checksum              10303
_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 'CMW 04-057 BuZnTsAq'
_olex2_submission_special_instructions 'No special instructions were received'