Reactions of osmapyridinium with terminal alkynes
Wei, Yuanqing; Zhou, Xiaoxi; Hong, Guangning; Chen, Zhixin; Zhang, Hong; Xia, Haiping; Organic Chemistry Frontiers 2 (2015) 560–; doi:10.1039/C5QO00052A

data_1553115
_publ_section_title
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 Reactions of osmapyridinium with terminal alkynes
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_journal_issue                   5
_journal_name_full               'Organic Chemistry Frontiers'
_journal_page_first              560
_journal_paper_doi               10.1039/C5QO00052A
_journal_volume                  2
_journal_year                    2015
_chemical_formula_moiety         'C48 H40 Cl N3 O Os P, 2(C H2 Cl2), B F4'
_chemical_formula_sum            'C50 H43 B Cl5 F4 N3 O Os P'
_chemical_formula_weight         1187.10
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-11-14
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2015-02-11 deposited with the CCDC.
2015-03-26 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.0230(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.0746(3)
_cell_length_b                   18.8448(3)
_cell_length_c                   20.9677(4)
_cell_measurement_reflns_used    8087
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      0
_cell_volume                     4771.06(17)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'multiwire proportional'
_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  0.0945
_diffrn_reflns_av_unetI/netI     0.0642
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            70908
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.11
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.044
_exptl_absorpt_correction_T_max  0.401
_exptl_absorpt_correction_T_min  0.175
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2356
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.3
_refine_diff_density_max         2.133
_refine_diff_density_min         -2.640
_refine_diff_density_rms         0.219
_refine_ls_extinction_coef       0.0029(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.170
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     598
_refine_ls_number_reflns         10901
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.170
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0526
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1054P)^2^+3.6588P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1396
_refine_ls_wR_factor_ref         0.1954
_reflns_number_gt                8348
_reflns_number_total             10901
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5qo00052a2.cif
_cod_data_source_block           1
_cod_database_code               1553115
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H1(0.034) H23(0.094) H11(0.042) H22(0.058) H12(0.045) H15(0.046)
 H14(0.052) H5A(0.058) H5B(0.058) H5C(0.058) H303(0.049) H304(0.059)
 H306(0.044) H305(0.054) H26(0.061) H325(0.074) H326(0.056) H25(0.092)
 H322(0.057) H324(0.084) H24(0.109) H323(0.074) H313(0.054) H1A(0.029)
 H34(0.042) H31(0.047) H6(0.04) H37(0.042) H312(0.042) H314(0.059) H39(0.047)
 H315(0.049) H33(0.056) H40(0.048) H316(0.043) H38(0.049) H1SA(0.075)
 H1SB(0.075) H32(0.055) H2SA(0.097) H2SB(0.097) H16A(0.1) H16B(0.1) H16C(0.1)
 Fixed X: H1(0.7284) H23(1.1259) H11(0.9861) H22(0.9867) H12(1.1092)
 H15(1.1521) H14(1.2744) H5A(0.9135) H5B(0.9977) H5C(0.8858) H303(0.4789)
 H304(0.4112) H306(0.6628) H305(0.4964) H26(1.073) H325(0.9319) H326(0.8359)
 H25(1.2153) H322(0.952) H324(1.0421) H24(1.2394) H323(1.0502) H313(0.5847)
 H1A(0.7742) H34(0.6335) H31(0.7832) H6(0.926) H37(0.5301) H312(0.6185)
 H314(0.7186) H39(0.4121) H315(0.8829) H33(0.743) H40(0.512) H316(0.9139)
 H38(0.4192) H1SA(0.5365) H1SB(0.5405) H32(0.8112) H2SA(1.6609) H2SB(1.7129)
 H16A(1.1976) H16B(1.3262) H16C(1.2711)
 Fixed Y: H1(3.6276) H23(3.5266) H11(3.5888) H22(3.566) H12(3.6723)
 H15(3.5765) H14(3.6612) H5A(3.6644) H5B(3.6557) H5C(3.696) H303(3.5414)
 H304(3.5106) H306(3.3755) H305(3.4242) H26(3.4202) H325(3.4382) H326(3.4667)
 H25(3.3818) H322(3.2866) H324(3.3386) H24(3.4334) H323(3.2629) H313(3.1855)
 H1A(3.4081) H34(3.4523) H31(3.6165) H6(3.4714) H37(3.3723) H312(3.2945)
 H314(3.1332) H39(3.2955) H315(3.1918) H33(3.5435) H40(3.3804) H316(3.303)
 H38(3.2916) H1SA(3.8052) H1SB(3.7222) H32(3.6277) H2SA(3.5698) H2SB(3.6346)
 H16A(3.7839) H16B(3.7943) H16C(3.7253)
 Fixed Z: H1(-0.2037) H23(-0.3932) H11(-0.0317) H22(-0.3266) H12(0.0063) H15(-
 0.1963) H14(-0.1599) H5A(-0.2833) H5B(-0.2269) H5C(-0.216) H303(-0.2558) H304(-
 0.356) H306(-0.3809) H305(-0.4167) H26(-0.1975) H325(-0.4769) H326(-0.3849)
 H25(-0.2639) H322(-0.3034) H324(-0.4808) H24(-0.3622) H323(-0.3958) H313(-
 0.2238) H1A(-0.1202) H34(0.0677) H31(-0.0684) H6(-0.0601) H37(0.0223) H312(-
 0.2686) H314(-0.1599) H39(-0.142) H315(-0.1391) H33(0.1081) H40(-0.1953) H316(-
 0.1832) H38(-0.0318) H1SA(-0.1399) H1SB(-0.1357) H32(0.0398) H2SA(0.6081)
 H2SB(0.572) H16A(0.0048) H16B(0.0096) H16C(0.0369)
;
_olex2_submission_special_instructions 'No special instructions were received'