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_4510862
_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         'C23 H36 K N2 O9 Os, C3 H6 O'
_chemical_formula_sum            'C26 H42 K N2 O10 Os'
_chemical_formula_weight         771.92
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-08-04
_audit_creation_method
;
  Olex2 1.1-beta
  (compiled 2011.02.15 svn.r1672, GUI svn.r3494)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 91.9260(19)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.66010(14)
_cell_length_b                   17.5692(3)
_cell_length_c                   26.7739(6)
_cell_measurement_reflns_used    13656
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      33.3352
_cell_measurement_theta_min      2.5557
_cell_volume                     3131.11(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.3 (release 07-12-2010 CrysAlis171 .NET)
(compiled Dec  7 2010,09:24:43)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.3 (release 07-12-2010 CrysAlis171 .NET)
(compiled Dec  7 2010,09:24:43)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.3 (release 07-12-2010 CrysAlis171 .NET)
(compiled Dec  7 2010,09:24:43)
;
_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  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
'A short history of SHELX (Sheldrick, 2007)/Bruker'
_diffrn_ambient_temperature      120.0
_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 -101.00   -4.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.3337  -38.0000   30.0000 194

  2 omega -101.00  -46.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.3337 -168.0000  157.0000 110

  3 omega  -74.00  -47.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.3337    0.0000 -120.0000 54

  4 omega   -1.00   45.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.3337    0.0000 -120.0000 92

  5 omega  -83.00  -22.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.3337  130.0000  139.0000 122

  6 omega -101.00   -3.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.3337  -38.0000 -180.0000 196

  7 omega  -98.00    2.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.3337  -77.0000  -30.0000 200

  8 omega  -98.00   -2.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.3337  -77.0000  150.0000 192

  9 omega   56.00  105.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       28.9587  179.0000  120.0000 98
;
_diffrn_measurement_device       '3-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       \w-scan
_diffrn_orient_matrix_UB_11      -0.0160286000
_diffrn_orient_matrix_UB_12      -0.0387617000
_diffrn_orient_matrix_UB_13      0.0060984000
_diffrn_orient_matrix_UB_21      -0.0026018000
_diffrn_orient_matrix_UB_22      -0.0094312000
_diffrn_orient_matrix_UB_23      -0.0257551000
_diffrn_orient_matrix_UB_31      0.1053861000
_diffrn_orient_matrix_UB_32      -0.0061633000
_diffrn_orient_matrix_UB_33      0.0011645000
_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  0.0380
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            42736
_diffrn_reflns_theta_full        29.50
_diffrn_reflns_theta_max         29.50
_diffrn_reflns_theta_min         2.56
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_source_type              'sealed tube'
_exptl_absorpt_coefficient_mu    4.259
_exptl_absorpt_correction_T_max  0.779
_exptl_absorpt_correction_T_min  0.257
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.3 (release 07-12-2010 CrysAlis171 .NET)
(compiled Dec  7 2010,09:24:43)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'metallic dark brown'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.637
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1548
_exptl_crystal_size_max          0.4373
_exptl_crystal_size_mid          0.2931
_exptl_crystal_size_min          0.059
_refine_diff_density_max         2.259
_refine_diff_density_min         -1.368
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.181
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     384
_refine_ls_number_reflns         8698
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.181
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0421
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+35.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0927
_refine_ls_wR_factor_ref         0.0940
_reflns_number_gt                8161
_reflns_number_total             8698
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg4016178_si_001.cif
_cod_data_source_block           Os2b_dbl26
_cod_depositor_comments
'Adding full bibliography for 4510860--4510862.cif.'
_cod_database_code               4510862
_chemical_oxdiff_formula         'C26 H41 K1 N2 O10 Os1'
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.44