Os(VI)O2/K Metal‒Organic Frameworks: Infinite Chain, Grid, and Porous Networks
Eckshtain-Levi, Meital; Yufit, Dmitry; Shimon, Linda J. W.; Kirillov, Alexander M.; Benisvy, Laurent; Crystal Growth & Design 14 (2014) 2703–; doi:10.1021/cg4016178

data_4510861
_publ_section_title
;
 Os(VI)O2/K Metal--Organic Frameworks: Infinite Chain, Grid, and Porous
 Networks
;
_journal_issue                   6
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              2703
_journal_paper_doi               10.1021/cg4016178
_journal_volume                  14
_journal_year                    2014
_chemical_formula_moiety         'C16 H21 K2 N2 O7 Os, 5(C H4 O)'
_chemical_formula_sum            'C21 H40 K2 N2 O12 Os'
_chemical_formula_weight         780.95
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-09-18
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 100.3064(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.3502(2)
_cell_length_b                   7.10564(11)
_cell_length_c                   30.6426(4)
_cell_measurement_reflns_used    14547
_cell_measurement_temperature    120.0(2)
_cell_measurement_theta_max      33.0449
_cell_measurement_theta_min      2.6970
_cell_volume                     2859.91(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_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
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard, H. Puschmann, 
in preparation (2013)
;
_diffrn_ambient_temperature      120.0(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 16.1511
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega -100.00   -4.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.3213  -38.0000   90.0000 192

  2 omega -100.00   -9.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.3213  -38.0000    0.0000 182

  3 omega   66.00  100.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       27.9463 -152.0000  -21.0000 68

  4 omega   68.00   96.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       27.9463  179.0000   60.0000 56

  5 omega  -97.00    3.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.3213  -77.0000  -90.0000 200

  6 omega -104.00  -32.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.3213  179.0000 -180.0000 144

  7 omega  -50.00   45.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.3213   38.0000   60.0000 190

  8 omega  -50.00   45.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.3213   38.0000 -180.0000 190

  9 omega   56.00  104.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       27.9463  179.0000  -60.0000 96

 10 omega   56.00  104.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       27.9463  179.0000 -180.0000 96
;
_diffrn_measurement_device       '3-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       \w-scan
_diffrn_orient_matrix_UB_11      -0.0099414000
_diffrn_orient_matrix_UB_12      -0.0100606000
_diffrn_orient_matrix_UB_13      -0.0234060000
_diffrn_orient_matrix_UB_21      0.0529588000
_diffrn_orient_matrix_UB_22      0.0045334000
_diffrn_orient_matrix_UB_23      -0.0002662000
_diffrn_orient_matrix_UB_31      0.0034257000
_diffrn_orient_matrix_UB_32      -0.0992177000
_diffrn_orient_matrix_UB_33      0.0023715000
_diffrn_radiation_collimation    monochromator
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_xray_symbol    Mo
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            42187
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         2.70
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_source_current           35
_diffrn_source_type              'sealed tube'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    4.811
_exptl_absorpt_correction_T_max  0.857
_exptl_absorpt_correction_T_min  0.423
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.814
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.2892
_exptl_crystal_size_mid          0.1224
_exptl_crystal_size_min          0.0359
_refine_diff_density_max         1.234
_refine_diff_density_min         -1.091
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         7611
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0254
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0230P)^2^+3.8000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0552
_refine_ls_wR_factor_ref         0.0567
_reflns_number_gt                6921
_reflns_number_total             7611
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg4016178_si_001.cif
_cod_data_source_block           Os2A_dbl27fin
_cod_depositor_comments
'Adding full bibliography for 4510860--4510862.cif.'
_cod_original_cell_volume        2859.92(8)
_cod_database_code               4510861
_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) groups
2. Restrained distances
 O5-H5
 0.85 with sigma of 0.01
 O5S-H5S
 0.85 with sigma of 0.01
 C16-H5
 1.888401 with sigma of 0.02
 C5S-H5S
 1.972934 with sigma of 0.02
3. Others
 Fixed Sof: Os1(0.99) O5S(0.7) H5S(0.7) C5S(0.7) H5SA(0.7) H5SB(0.7) H5SC(0.7)
 O6S(0.3) H6S(0.3) C6S(0.3) H6SA(0.3) H6SB(0.3) H6SC(0.3) Os1A(0.01)
4.a Riding coordinates:
 O4S(H4S), C4S(H4SA,H4SB,H4SC)
4.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C15(H15A,H15B), C16(H16A,H16B)
4.c Me refined with riding coordinates:
 C2S(H2SA,H2SB,H2SC)
4.d Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9)
4.e Idealised Me refined as rotating group:
 C1S(H1SA,H1SB,H1SC), C5S(H5SA,H5SB,H5SC), C11(H11A,H11B,H11C), C12(H12A,H12B,
 H12C), C13(H13A,H13B,H13C), C6S(H6SA,H6SB,H6SC), C3S(H3SA,H3SB,H3SC)
4.f Idealised tetrahedral OH refined as rotating group:
 O6S(H6S)
;