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_1553114
_publ_section_title
;
 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_formula_moiety
'C56 H48 Cl2 N O Os P2, B F4, 2(H2 O), 0.25(C H Cl3)'
_chemical_formula_sum            'C56.25 H52.25 B Cl2.75 F4 N O3 Os P2'
_chemical_formula_weight         1226.68
_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             2014-11-27
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.25 svn.r3098 for OlexSys, GUI svn.r4951)
;
_audit_update_record
;
2014-12-10 deposited with the CCDC.
2015-03-26 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 98.5760(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.9299(3)
_cell_length_b                   14.1946(3)
_cell_length_c                   33.0235(7)
_cell_measurement_temperature    153(2)
_cell_volume                     5529.7(2)
_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      153(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  0.0800
_diffrn_reflns_av_unetI/netI     0.0528
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            62557
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.08
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.553
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark violet'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2458
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Chloroform, n-hexane'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.144
_refine_diff_density_min         -1.296
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         9691
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0694
_refine_ls_R_factor_gt           0.0566
_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^)+(0.0855P)^2^+36.6174P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1635
_refine_ls_wR_factor_ref         0.1720
_reflns_number_gt                8011
_reflns_number_total             9691
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5qo00052a2.cif
_cod_data_source_block           1
_cod_database_code               1553114
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C1S) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: Cl1C(0.25) Cl1B(0.25) Cl1A(0.25) C1S(0.25) H1S(0.25)
4.a Riding coordinates:
 O1A(H1AA,H1AB), O1B(H1BA,H1BB)
4.b Ternary CH refined with riding coordinates:
 C6(H6), C1(H1A), C1S(H1S)
4.c Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B)
4.d Me refined with riding coordinates:
 C5(H5A,H5B,H5C)
4.e Aromatic/amide H refined with riding coordinates:
 N1(H1), C312(H312), C343(H343), C316(H316), C315(H315), C336(H336),
 C322(H322), C352(H352), C342(H342), C12(H12), C22(H22), C326(H326), C325(H325),
  C314(H314), C346(H346), C323(H323), C313(H313), C345(H345), C23(H23),
 C26(H26), C306(H306), C302(H302), C24(H24), C14(H14), C324(H324), C15(H15),
 C25(H25), C344(H344), C305(H305), C335(H335), C304(H304), C303(H303),
 C332(H332), C334(H334), C333(H333), C353(H353), C356(H356), C354(H354),
 C355(H355), C16(H16), C13(H13)
;
_olex2_submission_special_instructions 'No special instructions were received'