Dynamics of soft nanomaterials captured by transmission electron microscopy in liquid water.
Proetto, Maria T.; Rush, Anthony M.; Chien, Miao-Ping; Abellan Baeza, Patricia; Patterson, Joseph P.; Thompson, Matthew P.; Olson, Norman H.; Moore, Curtis E.; Rheingold, Arnold L.; Andolina, Christopher; Millstone, Jill; Howell, Stephen B.; Browning, Nigel D.; Evans, James E.; Gianneschi, Nathan C.; Journal of the American Chemical Society 136 (2014) 1162–1165; doi:10.1021/ja408513m

data_4120482
_publ_section_title
;
 Dynamics of soft nanomaterials captured by transmission electron
 microscopy in liquid water.
;
_journal_issue                   4
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1162
_journal_page_last               1165
_journal_paper_doi               10.1021/ja408513m
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'C17 H25 N3 O5 Pt'
_chemical_formula_sum            'C17 H25 N3 O5 Pt'
_chemical_formula_weight         546.49
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-07-22
_audit_creation_method
;
  Olex2 1.2-beta
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.0050(3)
_cell_length_b                   9.2447(3)
_cell_length_c                   34.6234(8)
_cell_measurement_reflns_used    9934
_cell_measurement_temperature    100
_cell_measurement_theta_max      68.152
_cell_measurement_theta_min      2.552
_cell_volume                     3522.51(17)
_computing_cell_refinement       'SAINT v8.30C (Bruker, 2013)'
_computing_data_collection       'Bruker APEX2 v2011.4-0 (Bruker, 2011)'
_computing_data_reduction        'SAINT v8.30C (Bruker, 2013)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XT, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX CCD'
_diffrn_detector_area_resol_mean 8.0
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker X8 APEX'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Double Bounce Multilayer Mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0538
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            25898
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        68.000
_diffrn_reflns_theta_max         68.330
_diffrn_reflns_theta_min         2.552
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Bruker FR-591'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    15.213
_exptl_absorpt_correction_T_max  0.1665
_exptl_absorpt_correction_T_min  0.0569
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1134 before and 0.0638 after correction.
The Ratio of minimum to maximum transmission is 0.3417.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            Colorless
_exptl_crystal_colour_primary    Colorless
_exptl_crystal_density_diffrn    2.061
_exptl_crystal_description       Needle
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.097
_exptl_crystal_size_mid          0.013
_exptl_crystal_size_min          0.005
_refine_diff_density_max         2.787
_refine_diff_density_min         -1.915
_refine_diff_density_rms         0.212
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.269
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         3127
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.263
_refine_ls_R_factor_all          0.0946
_refine_ls_R_factor_gt           0.0745
_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^)+179.3957P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1651
_refine_ls_wR_factor_ref         0.1731
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2146
_reflns_number_total             3127
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja408513m_si_007.cif
_cod_data_source_block           Gian04
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/usr/data/users/saulius/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_database_code               4120482
_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) groups,
  All N(H,H,H,H) groups
2. Restrained distances
 C11-C12B = C11-C15 = C11-C15B = C11-C12 = C15B-C14 = C15-C14 = C13-C14 = C13-
 C12 = C13B-C14 = C13B-C12B
 1.54 with sigma of 0.005
 C17-C13B = C15B-C16B
 1.54 with sigma of 0.005
 C17-C16B
 1.4 with sigma of 0.005
 C13-C17 = C15-C16
 1.54 with sigma of 0.005
 C17-C16
 1.4 with sigma of 0.005
 C7B-C8B = C7-C8 = C9B-C8B = C9B-C8 = C6B-C7 = C6B-C7B = C6B-C5 = C6B-C5B = C4-
 C5 = C4B-C5B = C9B-C4B = C9B-C4
 1.54 with sigma of 0.005
 N2-C5B = N1-C4B
 1.4 with sigma of 0.005
 N1-C4 = N2-C5
 1.4 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(C11) = Uanis(C12) = Uanis(C15) = Uanis(C17) = Uanis(C13) = Uanis(C16) = Uanis(C14) = Uanis(C16B) = Uanis(C12B) = Uanis(C15B) = Uanis(C13B)
Uanis(N2) = Uanis(C5) = Uanis(C5B) = Uanis(C4B) = Uanis(C4) = Uanis(N1) = Uanis(C9B) = Uanis(C8B) = Uanis(C7) = Uanis(C7B) = Uanis(C8) = Uanis(C6B)
4. Others
 Fixed Sof: H1AA(0.5) H1AB(0.5) H1BC(0.5) H1BD(0.5) H2AA(0.5) H2AB(0.5)
 H2BC(0.5) H2BD(0.5) C4(0.5) H4(0.5) C4B(0.5) H4B(0.5) C5(0.5) H5(0.5) C5B(0.5)
 H5B(0.5) H6BA(0.5) H6BB(0.5) H6BC(0.5) H6BD(0.5) C7(0.5) H7A(0.5) H7B(0.5)
 C7B(0.5) H7BA(0.5) H7BB(0.5) C8(0.5) H8A(0.5) H8B(0.5) C8B(0.5) H8BA(0.5)
 H8BB(0.5) H9BC(0.5) H9BD(0.5) H9BA(0.5) H9BB(0.5) H11(0.5) H11A(0.5) C12(0.5)
 H12A(0.5) H12B(0.5) C12B(0.5) H12C(0.5) H12D(0.5) C13(0.5) H13(0.5) C13B(0.5)
 H13B(0.5) H14A(0.5) H14B(0.5) H14C(0.5) H14D(0.5) C15(0.5) H15(0.5) C15B(0.5)
 H15B(0.5) C16(0.5) H16(0.5) C16B(0.5) H16B(0.5) H17(0.5) H17A(0.5)
5.a Ternary CH refined with riding coordinates:
 C2(H2), C4(H4), C4B(H4B), C5(H5), C5B(H5B), C11(H11), C11(H11A), C13(H13),
 C13B(H13B), C15(H15), C15B(H15B)
5.b Secondary CH2 refined with riding coordinates:
 N1(H1AA,H1AB), N1(H1BC,H1BD), N2(H2AA,H2AB), N2(H2BC,H2BD), C6B(H6BA,H6BB),
 C6B(H6BC,H6BD), C7(H7A,H7B), C7B(H7BA,H7BB), C8(H8A,H8B), C8B(H8BA,H8BB),
 C9B(H9BC,H9BD), C9B(H9BA,H9BB), C12(H12A,H12B), C12B(H12C,H12D), C14(H14A,
 H14B), C14(H14C,H14D)
5.c Aromatic/amide H refined with riding coordinates:
 N3(H3), C16(H16), C16B(H16B), C17(H17), C17(H17A)
;
_shelx_estimated_absorpt_t_max   0.928
_shelx_estimated_absorpt_t_min   0.320
_shelx_hkl_checksum              49297
_shelx_res_checksum              71916
_shelxl_version_number           2013-2