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_4510860
_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
;
C17 H24 K N O5 Os, 0.5(H2 O), 0.25(C6 H14), 0.5(C3 H6 O), 
0.25(C H4 O),  0.5(OH), 0.125 (O)
;
_chemical_formula_sum            'C20.25 H33 K N O6.88 Os'
_chemical_formula_weight         629.78
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-10-24
_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                 107.569(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   34.5483(15)
_cell_length_b                   10.6845(5)
_cell_length_c                   27.5819(11)
_cell_measurement_reflns_used    84777
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.49
_cell_measurement_theta_min      2.49
_cell_volume                     9706.4(7)
_computing_cell_refinement       'Bruker Apex2'
_computing_data_collection       'Bruker Apex2'
_computing_data_reduction        'Bruker Apex2'
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker KappaApex2 CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            79452
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         2.00
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    5.464
_exptl_absorpt_correction_T_max  0.9474
_exptl_absorpt_correction_T_min  0.4079
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker APEX2'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.724
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4984
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.535
_refine_diff_density_min         -0.959
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     563
_refine_ls_number_reflns         12911
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0257
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+45.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0537
_refine_ls_wR_factor_ref         0.0563
_reflns_number_gt                11171
_reflns_number_total             12911
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg4016178_si_001.cif
_cod_data_source_block           Os1_oslha
_cod_depositor_comments
'Adding full bibliography for 4510860--4510862.cif.'
_cod_database_code               4510860
_olex2_refinement_description
;
1. Others
 Fixed Sof: C15B(0.5) H15A(0.5) H15B(0.5) H15C(0.5) C16B(0.5) H16A(0.5)
 H16B(0.5) H16C(0.5) C17B(0.5) H17A(0.5) H17B(0.5) H17C(0.5) C28(0.6) H28A(0.6)
 H28B(0.6) H28C(0.6) C29(0.6) H29A(0.6) H29B(0.6) H29C(0.6) C30(0.6) H30A(0.6)
 H30B(0.6) H30C(0.6) C28A(0.4) H28D(0.4) H28E(0.4) H28F(0.4) C29A(0.4)
 H29D(0.4) H29E(0.4) H29F(0.4) C30A(0.4) H30D(0.4) H30E(0.4) H30F(0.4)
 H1SD(0.5) H1SE(0.5) H1SF(0.5) H1SA(0.5) H1SB(0.5) H1SC(0.5) C3SB(0.5)
 H3SA(0.5) H3SB(0.5) O2S(0.3) H2S(0.3) C15A(0.5) H15D(0.5) H15E(0.5) H15F(0.5)
 C17A(0.5) H17D(0.5) H17E(0.5) H17F(0.5) C16A(0.5) H16D(0.5) H16E(0.5)
 H16F(0.5) C2SB(0.5) H2SA(0.5) H2SB(0.5) C2SA(0.5) H2SC(0.5) H2SD(0.5)
 C3SA(0.5) H3SC(0.5) H3SD(0.5) O1S(0.2) H1S(0.2) O3S(0.25) C4S(0.2) H4SA(0.2)
 H4SB(0.2) H4SC(0.2) C5S(0.3) H5SA(0.3) H5SB(0.3) H5SC(0.3)
 Fixed Uiso: H4(0.03) H3(0.021) H5(0.019) H8A(0.033) H8B(0.033) H9A(0.031)
 H9B(0.031) H11A(0.037) H11B(0.037) H11C(0.037) H12A(0.039) H12B(0.039)
 H12C(0.039) H13A(0.036) H13B(0.036) H13C(0.036) H15A(0.053) H15B(0.053)
 H15C(0.053) H16A(0.066) H16B(0.066) H16C(0.066) H17A(0.015) H17B(0.015)
 H17C(0.015) H20(0.021) H22(0.02) H25A(0.025) H25B(0.025) H26A(0.024)
 H26B(0.024) H28A(0.055) H28B(0.055) H28C(0.055) H29A(0.058) H29B(0.058)
 H29C(0.058) H30A(0.055) H30B(0.055) H30C(0.055) H32A(0.037) H32B(0.037)
 H32C(0.037) H33A(0.036) H33B(0.036) H33C(0.036) H34A(0.038) H34B(0.038)
 H34C(0.038) H36A(0.05) H36B(0.05) H36C(0.05) H37A(0.06) H37B(0.06) H37C(0.06)
 H14A(0.073) H14B(0.073) H28D(0.048) H28E(0.048) H28F(0.048) H29D(0.065)
 H29E(0.065) H29F(0.065) H30D(0.068) H30E(0.068) H30F(0.068) H1SD(0.146)
 H1SE(0.146) H1SF(0.146) H1SA(0.146) H1SB(0.146) H1SC(0.146) H3SA(0.053)
 H3SB(0.053) H2S(0.048) H15D(0.05) H15E(0.05) H15F(0.05) H17D(0.084)
 H17E(0.084) H17F(0.084) H16D(0.039) H16E(0.039) H16F(0.039) H2SA(0.067)
 H2SB(0.067) H2SC(0.087) H2SD(0.087) H3SC(0.079) H3SD(0.079) H1S(0.052)
 H4SA(0.067) H4SB(0.067) H4SC(0.067) H5SA(0.067) H5SB(0.067) H5SC(0.067)
 Fixed X: H4(0.6516) H3(0.5588) H5(0.6776) H8A(0.7806) H8B(0.7754) H9A(0.801)
 H9B(0.7678) H11A(0.5286) H11B(0.5767) H11C(0.5479) H12A(0.4929) H12B(0.51)
 H12C(0.5162) H13A(0.5859) H13B(0.5377) H13C(0.5592) H15A(0.667) H15B(0.6394)
 H15C(0.6588) H16A(0.5732) H16B(0.5907) H16C(0.62) H17A(0.5657) H17B(0.5613)
 H17C(0.5449) H20(0.8561) H22(0.9159) H25A(0.7222) H25B(0.7331) H26A(0.6682)
 H26B(0.6794) H28A(0.9665) H28B(0.9868) H28C(0.9711) H29A(0.9328) H29B(0.9513)
 H29C(0.9032) H30A(0.8913) H30B(0.9391) H30C(0.9151) H32A(0.9297) H32B(0.8988)
 H32C(0.9044) H33A(0.8585) H33B(0.9058) H33C(0.881) H34A(0.8244) H34B(0.8074)
 H34C(0.8335) H36A(0.8704) H36B(0.8612) H36C(0.905) H37A(0.9033) H37B(0.897)
 H37C(0.8635) H14A(0.6405) H14B(0.6292) H28D(0.9712) H28E(0.98) H28F(0.9545)
 H29D(0.8939) H29E(0.9274) H29F(0.8856) H30D(0.9138) H30E(0.9558) H30F(0.9528)
 H1SD(0.4708) H1SE(0.4853) H1SF(0.5182) H1SA(0.4834) H1SB(0.472) H1SC(0.5186)
 H3SA(0.4758) H3SB(0.5237) H2S(0.9312) H15D(0.6667) H15E(0.633) H15F(0.6405)
 H17D(0.587) H17E(0.5719) H17F(0.5521) H16D(0.5861) H16E(0.6067) H16F(0.6345)
 H2SA(0.4618) H2SB(0.5094) H2SC(0.509) H2SD(0.4621) H3SC(0.4805) H3SD(0.5277)
 H1S(0.9285) H4SA(0.944) H4SB(0.9655) H4SC(0.9909) H5SA(0.9915) H5SB(1.0009)
 H5SC(0.9798)
 Fixed Y: H4(0.5784) H3(0.355) H5(0.3825) H8A(0.4046) H8B(0.544) H9A(0.424)
 H9B(0.3166) H11A(0.5819) H11B(0.5975) H11C(0.6217) H12A(0.4059) H12B(0.4467)
 H12C(0.3062) H13A(0.3701) H13B(0.3699) H13C(0.2626) H15A(0.2566) H15B(0.2898)
 H15C(0.3997) H16A(0.159) H16B(0.1365) H16C(0.1236) H17A(0.456) H17B(0.337)
 H17C(0.3305) H20(0.456) H22(0.267) H25A(0.5991) H25B(0.722) H26A(0.6705)
 H26B(0.525) H28A(0.4569) H28B(0.3367) H28C(0.3298) H29A(0.1375) H29B(0.1432)
 H29C(0.1322) H30A(0.3214) H30B(0.3285) H30C(0.4502) H32A(0.2444) H32B(0.1348)
 H32C(0.1737) H33A(0.4755) H33B(0.447) H33C(0.3808) H34A(0.1657) H34B(0.2971)
 H34C(0.2095) H36A(0.4415) H36B(0.3531) H36C(0.416) H37A(0.6714) H37B(0.6581)
 H37C(0.728) H14A(0.7989) H14B(0.7254) H28D(0.3329) H28E(0.263) H28F(0.194)
 H29D(0.1882) H29E(0.2558) H29F(0.3257) H30D(0.5109) H30E(0.4527) H30F(0.5141)
 H1SD(0.022) H1SE(0.1632) H1SF(0.0553) H1SA(0.0442) H1SB(0.1536) H1SC(0.1193)
 H3SA(-0.0742) H3SB(-0.0498) H2S(0.6946) H15D(0.3364) H15E(0.349) H15F(0.462)
 H17D(0.4766) H17E(0.3537) H17F(0.3913) H16D(0.147) H16E(0.1491) H16F(0.1497)
 H2SA(0.1412) H2SB(0.1743) H2SC(-0.0825) H2SD(-0.0507) H3SC(0.1126)
 H3SD(0.0842) H1S(0.9349) H4SA(0.7401) H4SB(0.7665) H4SC(0.7797) H5SA(0.7552)
 H5SB(0.7419) H5SC(0.8662)
 Fixed Z: H4(0.3331) H3(0.5243) H5(0.6008) H8A(0.5284) H8B(0.5054) H9A(0.4514)
 H9B(0.4478) H11A(0.385) H11B(0.4084) H11C(0.4432) H12A(0.4075) H12B(0.4659)
 H12C(0.4495) H13A(0.3811) H13B(0.3562) H13C(0.3956) H15A(0.6612) H15B(0.6967)
 H15C(0.6721) H16A(0.5804) H16B(0.6404) H16C(0.6055) H17A(0.6184) H17B(0.6516)
 H17C(0.5909) H20(0.7324) H22(0.8582) H25A(0.6953) H25B(0.7304) H26A(0.729)
 H26B(0.7379) H28A(0.8028) H28B(0.7858) H28C(0.8348) H29A(0.8029) H29B(0.7563)
 H29C(0.7457) H30A(0.6931) H30B(0.7015) H30C(0.7104) H32A(0.9384) H32B(0.9124)
 H32C(0.9701) H33A(0.9456) H33B(0.9568) H33C(0.9901) H34A(0.8973) H34B(0.91)
 H34C(0.9551) H36A(0.5413) H36B(0.5833) H36C(0.5938) H37A(0.6347) H37B(0.575)
 H37C(0.5945) H14A(0.2749) H14B(0.3117) H28D(0.8282) H28E(0.7813) H28F(0.8131)
 H29D(0.7204) H29E(0.7003) H29F(0.6964) H30D(0.7297) H30E(0.7273) H30F(0.779)
 H1SD(0.6073) H1SE(0.6215) H1SF(0.6251) H1SA(0.6337) H1SB(0.5921) H1SC(0.6195)
 H3SA(0.525) H3SB(0.5496) H2S(0.7048) H15D(0.6671) H15E(0.6958) H15F(0.6617)
 H17D(0.6402) H17E(0.6623) H17F(0.6039) H16D(0.5916) H16E(0.652) H16F(0.6149)
 H2SA(0.5288) H2SB(0.5467) H2SC(0.5767) H2SD(0.5501) H3SC(0.5028) H3SD(0.5302)
 H1S(0.7199) H4SA(0.7179) H4SB(0.777) H4SC(0.7374) H5SA(0.7143) H5SB(0.7746)
 H5SC(0.7463)
;