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_1553113
_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, 2(C H2 Cl2), B F4'
_chemical_formula_sum            'C58 H52 B Cl6 F4 N O Os P2'
_chemical_formula_weight         1330.65
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_audit_creation_date             2014-12-30
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4959)
;
_audit_update_record
;
2015-02-11 deposited with the CCDC.
2015-03-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.182(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.5731(8)
_cell_length_b                   19.6848(7)
_cell_length_c                   18.1839(9)
_cell_measurement_temperature    173(2)
_cell_volume                     5493.2(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.996
_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  0.1019
_diffrn_reflns_av_unetI/netI     0.0854
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            38256
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.020
_exptl_absorpt_coefficient_mu    2.727
_exptl_absorpt_correction_T_max  0.441
_exptl_absorpt_correction_T_min  0.212
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_description       plate
_exptl_crystal_F_000             2656
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         4.637
_refine_diff_density_min         -2.056
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     669
_refine_ls_number_reflns         9642
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0779
_refine_ls_R_factor_gt           0.0643
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1025P)^2^+14.8409P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1710
_refine_ls_wR_factor_ref         0.1873
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7791
_reflns_number_total             9642
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5qo00052a2.cif
_cod_data_source_block           1
_cod_database_code               1553113
_shelxl_version_number           2013-2
_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.a Ternary CH refined with riding coordinates:
 C1(H1A), C6(H6)
2.b Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C31(H31A,H31B)
2.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C353(H353), C336(H336), C26(H26), C23(H23), C332(H332), C16(H16),
 C322(H322), C12(H12), C13(H13), C362(H362), C326(H326), C364(H364), C324(H324),
  C14(H14), C22(H22), C366(H366), C365(H365), C25(H25), C335(H335), C363(H363),
 C323(H323), C333(H333), C325(H325), C312(H312), C334(H334), C314(H314),
 C313(H313), C352(H352), C356(H356), C342(H342), C354(H354), C355(H355),
 C346(H346), C345(H345), C343(H343), C344(H344), N1(H1), C315(H315), C316(H316)
2.d Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C27(H27A,H27B,H27C)
;
_shelx_res_checksum              72708
_shelx_hkl_checksum              27872
_olex2_submission_special_instructions 'No special instructions were received'