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_4129778
_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         '2(C27 H35 N4 O7.52 S3 Zn), 2(C16 H36 N)'
_chemical_formula_sum            'C86 H142 N10 O15 S6 Zn2'
_chemical_formula_weight         1879.19
_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             2015-11-05
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2015.10.28 svn.r3245 for OlexSys, GUI svn.r5128)
;
_cell_angle_alpha                92.9514(19)
_cell_angle_beta                 97.9613(18)
_cell_angle_gamma                109.1389(19)
_cell_formula_units_Z            1
_cell_length_a                   9.3583(12)
_cell_length_b                   13.4896(18)
_cell_length_c                   19.634(3)
_cell_measurement_reflns_used    9973
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.138
_cell_measurement_theta_min      2.398
_cell_volume                     2306.6(6)
_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 0.997
_diffrn_measured_fraction_theta_max 0.949
_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  0.0408
_diffrn_reflns_av_unetI/netI     0.0668
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            30794
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         31.162
_diffrn_reflns_theta_min         1.827
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           35
_diffrn_source_voltage           45
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.723
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6077
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1252 before and 0.0520 after correction.
The Ratio of minimum to maximum transmission is 0.8144.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_description       prism
_exptl_crystal_F_000             1004
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of diethyl ether and THF by vapor diffusion'
_exptl_crystal_size_max          0.781
_exptl_crystal_size_mid          0.444
_exptl_crystal_size_min          0.398
_refine_diff_density_max         2.569
_refine_diff_density_min         -1.172
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     662
_refine_ls_number_reflns         14175
_refine_ls_number_restraints     495
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.1204
_refine_ls_R_factor_gt           0.0864
_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^)+(0.0613P)^2^+9.5022P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1938
_refine_ls_wR_factor_ref         0.2157
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10044
_reflns_number_total             14175
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b10450_si_002.cif
_cod_data_source_block           cmw04-buzntso2h2xtal2
_cod_original_cell_volume        2306.5(5)
_cod_database_code               4129778
_shelx_estimated_absorpt_t_max   0.762
_shelx_estimated_absorpt_t_min   0.602
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H,H) groups
2. Restrained distances
 C42A-C41A
 1.52 with sigma of 0.005
 C43A-C42A
 1.52 with sigma of 0.005
 C43B-C42B = C42B-C41B
 1.52 with sigma of 0.005
 C43B-C41B
 2.51 with sigma of 0.01
 C41A-C40A
 1.52 with sigma of 0.005
 O2'-H2'
 0.999 with sigma of 0.002
 H1WA-O1W = O1W-H1WB
 0.995 with sigma of 0.02
 O1'-H1'
 0.995 with sigma of 0.002
 C41A-C40A \\sim C29A-C28A \\sim C33A-C32A \\sim C37A-C36A
 with sigma of 0.002
 Zn1-N3A \\sim Zn1-N3B
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
O1W \\sim O1': within 2A with sigma of 0.002 and sigma for terminal atoms of
0.002
Uanis(O1') \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(C28A) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.006
Uanis(N5A) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.006
Uanis(C21A) \\sim Ueq, Uanis(C25A) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
Uanis(S3A) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(O6A) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.006
Uanis(O7A) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.006
Uanis(C27A) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.006
Uanis(N3B) \\sim Ueq, Uanis(N3A) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.006
Uanis(S3A) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C23B) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C23A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C25B) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C24A) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.006
Uanis(O1W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(N5A) = Uanis(N5B)
Uanis(C28A) = Uanis(C28B)
Uanis(C40A) = Uanis(C40B)
Uanis(C36A) = Uanis(C36B)
Uanis(C32A) = Uanis(C32B)
Uanis(C29A) = Uanis(C29B)
Uanis(C41A) = Uanis(C41B)
Uanis(C37A) = Uanis(C37B)
Uanis(C33A) = Uanis(C33B)
Uanis(C30A) = Uanis(C30B)
Uanis(C42A) = Uanis(C42B)
Uanis(C38A) = Uanis(C38B)
Uanis(C34A) = Uanis(C34B)
Uanis(C31A) = Uanis(C31B)
Uanis(C43A) = Uanis(C43B)
Uanis(C39A) = Uanis(C39B)
Uanis(C35A) = Uanis(C35B)
Uanis(N3A) = Uanis(N3B)
Uanis(S3A) = Uanis(S3B)
Uanis(O7A) = Uanis(O7B)
Uanis(O6A) = Uanis(O6B)
Uanis(C21A) = Uanis(C21B)
Uanis(C24A) = Uanis(C24B)
Uanis(C27B) = Uanis(C27A)
Uanis(C22A) = Uanis(C22B)
Uanis(C26A) = Uanis(C26B)
Uiso(H1') = Uiso(H1WB)
4. Rigid body (RIGU) restrains
 O1', O2'
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N5B, C28B, C29B, C30B, C31B, C32B, C33B, C34B, C35B, C36B, C37B, C38B, C39B,
 C40B, C41B, C42B, C43B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 N5A, C28A, C29A, C30A, C31A, C32A, C33A, C34A, C35A, C36A, C37A, C38A, C39A,
 C40A, C41A, C42A, C43A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 S3A, O6A, O7A, N3A, C21A, C22A, C23A, C24A, C25A, C26A, C27A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 Zn1, O1', O2'
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 Zn1, O1', O1W
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Same fragment restrains
{N5B, 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
{N5A, C28A, C29A, C30A, C31A, C32A, C33A, C34A, C35A, C36A, C37A, C38A, C39A,
C40A, C41A, C42A, C43A}
{S3B, O6B, O7B, N3B, C21B, C22B, C23B, C24B, C25B, C26B, C27B} sigma for 1-2:
0.002, 1-3: 0.002
as
{S3A, O6A, O7A, N3A, C21A, C22A, C23A, C24A, C25A, C26A, C27A}
6. Others
 Sof(N5B)=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)=Sof(S3B)=Sof(O6B)=Sof(O7B)=Sof(N3B)=
 Sof(C21B)=Sof(C22B)=Sof(H22B)=Sof(C23B)=Sof(H23B)=Sof(C24B)=Sof(C25B)=
 Sof(H25B)=Sof(C26B)=Sof(H26B)=Sof(C27B)=Sof(H27D)=Sof(H27E)=Sof(H27F)=Sof(O1')=
 Sof(O2')=Sof(H2')=Sof(H1')=1-FVAR(1)
 Sof(N5A)=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)=Sof(S3A)=Sof(O6A)=Sof(O7A)=Sof(N3A)=
 Sof(C21A)=Sof(C22A)=Sof(H22A)=Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(C25A)=
 Sof(H25A)=Sof(C26A)=Sof(H26A)=Sof(C27A)=Sof(H27A)=Sof(H27B)=Sof(H27C)=Sof(O1W)=
 Sof(H1WA)=Sof(H1WB)=FVAR(1)
7.a Riding coordinates:
 O1W(H1WA,H1WB), O1W(H2')
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(H5A,H5B), C6(H6A,H6B)
7.c Aromatic/amide H refined with riding coordinates:
 C22A(H22A), C23A(H23A), C25A(H25A), C26A(H26A), C22B(H22B), C23B(H23B),
 C25B(H25B), C26B(H26B), C8(H8), C9(H9), C11(H11), C12(H12), C15(H15), C16(H16),
  C18(H18), C19(H19)
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), C27A(H27A,H27B,H27C), C27B(H27D,H27E,H27F), C13(H13A,
 H13B,H13C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              58951
_shelx_hkl_checksum              12845
_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 1-H2O2
_olex2_submission_special_instructions 'No special instructions were received'