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_4129776
_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         'C16 H36 N, C27 H37 N6 O6 S3 Zn'
_chemical_formula_sum            'C43 H73 N7 O6 S3 Zn'
_chemical_formula_weight         945.63
_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             2015-10-02
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                97.526(3)
_cell_angle_beta                 96.225(3)
_cell_angle_gamma                109.087(3)
_cell_formula_units_Z            2
_cell_length_a                   9.117(2)
_cell_length_b                   13.492(3)
_cell_length_c                   20.272(4)
_cell_measurement_reflns_used    9800
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.997
_cell_measurement_theta_min      2.381
_cell_volume                     2305.5(9)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2014.11 (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-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/4 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_av_unetI/netI     0.0547
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            33079
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         1.760
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           35
_diffrn_source_voltage           45
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.722
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6393
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1552 before and 0.0585 after correction.
The Ratio of minimum to maximum transmission is 0.8574.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_description       needle
_exptl_crystal_F_000             1012
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of DCM and ethanol by vapor diffusion'
_exptl_crystal_size_max          0.559
_exptl_crystal_size_mid          0.205
_exptl_crystal_size_min          0.155
_refine_diff_density_max         1.452
_refine_diff_density_min         -1.004
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     636
_refine_ls_number_reflns         10558
_refine_ls_number_restraints     319
_refine_ls_restrained_S_all      9.858
_refine_ls_R_factor_all          0.0954
_refine_ls_R_factor_gt           0.0713
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0699P)^2^+9.1452P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1624
_refine_ls_wR_factor_ref         0.1793
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8173
_reflns_number_total             10558
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b10450_si_002.cif
_cod_data_source_block           cmw04-088buzntsn2h4
_cod_database_code               4129776
_shelx_estimated_absorpt_t_max   0.896
_shelx_estimated_absorpt_t_min   0.688
_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. Restrained distances
 C42B-C41B
 1.52 with sigma of 0.005
 C33A-C32A
 1.52 with sigma of 0.005
 N5-H5 = N5-H5A
 0.975 with sigma of 0.005
 H6A-N6 = N6-H6D
 0.975 with sigma of 0.005
 H5-H5A
 1.55 with sigma of 0.04
 H6A-H6D
 1.553 with sigma of 0.04
 C40A-C32A \\sim C36A-C32A \\sim C32A-C28A \\sim C40A-C36A \\sim C40A-C28A
 with sigma of 0.005
 N7B-C40B \\sim N7B-C32B \\sim N7B-C28B \\sim N7B-C36B
 with sigma of 0.005
 C35A-C34A \\sim C43A-C42A \\sim C39A-C38A \\sim C31A-C30A
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(C40A) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(C42A) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C41A) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C33A) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(C32A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C36A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C31A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C21) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(N7A) = Uanis(N7B)
Uanis(C36A) = Uanis(C36B)
Uanis(C31A) = Uanis(C31B)
Uanis(C29A) = Uanis(C29B)
Uanis(C40A) = Uanis(C40B)
Uanis(C35A) = Uanis(C35B)
Uanis(C37B) = Uanis(C37A)
Uanis(C43A) = Uanis(C43B)
Uanis(C33B) = Uanis(C33A)
Uanis(C32B) = Uanis(C32A)
Uanis(C28A) = Uanis(C28B)
Uanis(C41A) = Uanis(C41B)
Uanis(C30A) = Uanis(C30B)
Uiso(H6D) = Uiso(H6A)
Uiso(H6A) = Uiso(H6D)
4. Rigid body (RIGU) restrains
 N7B, N7A, C28A, C32A, C36A, C40A, C29A, C33A, C28B, C37A, C41A, C36B, C37B,
 C30A, C34A, C29B, C32B, C40B, C38A, C42A, C38B, C31A, C35A, C30B, C33B, C41B,
 C39A, C43A, C39B, C31B, C34B, C42B, C35B, C43B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N5, N6
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Same fragment restrains
{N7B, C28B, C29B, C30B, C31B, C32B, C33B, C34B, C35B, C36B, C37B, C38B, C39B,
C40B, C41B, C42B, C43B} sigma for 1-2: 0.002, 1-3: 0.002
as
{N7A, C28A, C29A, C30A, C31A, C32A, C33A, C34A, C35A, C36A, C37A, C38A, C39A,
C40A, C41A, C42A, C43A}
6. Others
 Sof(N7B)=Sof(C28B)=Sof(H28C)=Sof(H28D)=Sof(C29B)=Sof(H29C)=Sof(H29D)=
 Sof(C30B)=Sof(H30C)=Sof(H30D)=Sof(C31B)=Sof(H31D)=Sof(H31E)=Sof(H31F)=
 Sof(C32B)=Sof(H32C)=Sof(H32D)=Sof(C33B)=Sof(H33C)=Sof(H33D)=Sof(C34B)=
 Sof(H34C)=Sof(H34D)=Sof(C35B)=Sof(H35D)=Sof(H35E)=Sof(H35F)=Sof(C36B)=
 Sof(H36C)=Sof(H36D)=Sof(C37B)=Sof(H37C)=Sof(H37D)=Sof(C38B)=Sof(H38C)=
 Sof(H38D)=Sof(C39B)=Sof(H39D)=Sof(H39E)=Sof(H39F)=Sof(C40B)=Sof(H40C)=
 Sof(H40D)=Sof(C41B)=Sof(H41C)=Sof(H41D)=Sof(C42B)=Sof(H42C)=Sof(H42D)=
 Sof(C43B)=Sof(H43D)=Sof(H43E)=Sof(H43F)=1-FVAR(1)
 Sof(N7A)=Sof(C28A)=Sof(H28A)=Sof(H28B)=Sof(C29A)=Sof(H29A)=Sof(H29B)=
 Sof(C30A)=Sof(H30A)=Sof(H30B)=Sof(C31A)=Sof(H31A)=Sof(H31B)=Sof(H31C)=
 Sof(C32A)=Sof(H32A)=Sof(H32B)=Sof(C33A)=Sof(H33A)=Sof(H33B)=Sof(C34A)=
 Sof(H34A)=Sof(H34B)=Sof(C35A)=Sof(H35A)=Sof(H35B)=Sof(H35C)=Sof(C36A)=
 Sof(H36A)=Sof(H36B)=Sof(C37A)=Sof(H37A)=Sof(H37B)=Sof(C38A)=Sof(H38A)=
 Sof(H38B)=Sof(C39A)=Sof(H39A)=Sof(H39B)=Sof(H39C)=Sof(C40A)=Sof(H40A)=
 Sof(H40B)=Sof(C41A)=Sof(H41A)=Sof(H41B)=Sof(C42A)=Sof(H42A)=Sof(H42B)=
 Sof(C43A)=Sof(H43A)=Sof(H43B)=Sof(H43C)=FVAR(1)
7.a Everything fixed:
 H6A, H6B
7.b Secondary CH2 refined with riding coordinates:
 C28A(H28A,H28B), C29A(H29A,H29B), C30A(H30A,H30B), C32A(H32A,H32B), C33A(H33A,
 H33B), C34A(H34A,H34B), C36A(H36A,H36B), C37A(H37A,H37B), C38A(H38A,H38B),
 C40A(H40A,H40B), C41A(H41A,H41B), C42A(H42A,H42B), C28B(H28C,H28D), C29B(H29C,
 H29D), C30B(H30C,H30D), C32B(H32C,H32D), C33B(H33C,H33D), C34B(H34C,H34D),
 C36B(H36C,H36D), C37B(H37C,H37D), C38B(H38C,H38D), C40B(H40C,H40D), C41B(H41C,
 H41D), C42B(H42C,H42D), C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B),
 C5(H5B,H5C), C6(H6C,H6D)
7.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C11(H11), C12(H12), C15(H15), C16(H16), C18(H18), C19(H19),
 C22(H22), C23(H23), C25(H25), C26(H26)
7.d Idealised Me refined as rotating group:
 C31A(H31A,H31B,H31C), C35A(H35A,H35B,H35C), C39A(H39A,H39B,H39C), C43A(H43A,
 H43B,H43C), C31B(H31D,H31E,H31F), C35B(H35D,H35E,H35F), C39B(H39D,H39E,H39F),
 C43B(H43D,H43E,H43F), C13(H13A,H13B,H13C), C20(H20A,H20B,H20C), C27(H27A,H27B,
 H27C)
;
_shelx_res_checksum              44953
_shelx_hkl_checksum              16522
_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 CMW04-088BuZnTsN2H4
_olex2_submission_special_instructions 'No special instructions were received'