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_1553116
_publ_section_title
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 Reactions of osmapyridinium with terminal alkynes
;
_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_absolute_configuration ad
_chemical_formula_moiety         'C51 H53 Cl2 N3 Os P, C H2 Cl2, B F4'
_chemical_formula_sum            'C52 H55 B Cl4 F4 N3 Os P'
_chemical_formula_weight         1171.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-02-07
_audit_creation_method
;
Olex2 1.2
(compiled 2014.12.26 svn.r3119 for OlexSys, GUI svn.r4975)
;
_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                 111.0040(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.3445(9)
_cell_length_b                   16.8974(6)
_cell_length_c                   16.1902(7)
_cell_measurement_temperature    173(2)
_cell_volume                     4940.5(4)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0439
_diffrn_reflns_av_unetI/netI     0.0763
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18915
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         3.25
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.884
_exptl_absorpt_correction_T_max  0.315
_exptl_absorpt_correction_T_min  0.137
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2352
_exptl_crystal_size_max          1.0
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.4
_refine_diff_density_max         1.433
_refine_diff_density_min         -1.148
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.005(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     596
_refine_ls_number_reflns         7754
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0344
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0304P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0737
_refine_ls_wR_factor_ref         0.0858
_reflns_number_gt                6954
_reflns_number_total             7754
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5qo00052a2.cif
_cod_data_source_block           1
_cod_database_code               1553116
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C35-C36
 1.54 with sigma of 0.02
 C32-C33
 1.54 with sigma of 0.02
 C32-N3
 1.47 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C37) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C34)
\\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C36) \\sim Ueq, Uanis(C35) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C45) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Ternary CH refined with riding coordinates:
 C42(H42), C32(H32)
4.b Secondary CH2 refined with riding coordinates:
 C100(H10A,H10B), C46(H46A,H46B), C47(H47A,H47B), C43(H43A,H43B), C44(H44A,
 H44B), C45(H45A,H45B), C37(H37A,H37B), C34(H34A,H34B), C35(H35A,H35B),
 C33(H33A,H33B), C36(H36A,H36B)
4.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C14(H14), C322(H322), C6(H6), C26(H26), C312(H312), C12(H12),
 C303(H303), C304(H304), C16(H16), C1(H1), C324(H324), C306(H306), C316(H316),
 C326(H326), C302(H302), C314(H314), C25(H25), C323(H323), C315(H315), C13(H13),
  C305(H305), C24(H24), C22(H22), C23(H23), C325(H325), N1(H1A), C313(H313)
4.d Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C)
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_olex2_submission_special_instructions 'No special instructions were received'