Conventional and unconventional alkyne activations by Ru and Os for unprecedented dimetalated quinolizinium complexes.
Yeung, Chi-Fung; Chung, Lai-Hon; Tse, Sheung-Ying; Shek, Hau-Lam; Tse, Man-Kit; Yiu, Shek-Man; Wong, Chun-Yuen; Chemical communications (Cambridge, England) 56 (2020) 8908–8911; doi:10.1039/d0cc03480k

data_7126879
_publ_section_title
;
 Conventional and unconventional alkyne activations by Ru and Os for
 unprecedented dimetalated quinolizinium complexes.
;
_journal_issue                   63
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              8908
_journal_page_last               8911
_journal_paper_doi               10.1039/d0cc03480k
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C65 H54 N P4 Ru, Cl O4, C H2 Cl2'
_chemical_formula_sum            'C66 H56 Cl3 N O4 P4 Ru'
_chemical_formula_weight         1258.41
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-09-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-05-05 deposited with the CCDC.	2020-07-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.7930(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.6796(2)
_cell_length_b                   19.9722(3)
_cell_length_c                   13.1880(2)
_cell_measurement_reflns_used    7339
_cell_measurement_temperature    223.4(8)
_cell_measurement_theta_max      71.7150
_cell_measurement_theta_min      10.0880
_cell_volume                     2974.36(8)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      223.4(8)
_diffrn_detector_area_resol_mean 16.1270
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0272
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13158
_diffrn_reflns_point_group_measured_fraction_full 0.730
_diffrn_reflns_point_group_measured_fraction_max 0.710
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.855
_diffrn_reflns_theta_min         4.113
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.781
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86443
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_description       block
_exptl_crystal_F_000             1292
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.705
_refine_diff_density_min         -0.522
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details
;
 Flack x determined using 2226 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.005(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     712
_refine_ls_number_reflns         8289
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0305
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0439P)^2^+0.8711P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0779
_refine_ls_wR_factor_ref         0.0788
_reflns_Friedel_coverage         0.402
_reflns_Friedel_fraction_full    0.446
_reflns_Friedel_fraction_max     0.420
_reflns_number_gt                8088
_reflns_number_total             8289
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc03480k2.cif
_cod_data_source_block           1q
_cod_depositor_comments
'Adding full bibliography for 7126879--7126885.cif.'
_cod_database_code               7126879
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C53(H53A,H53B), C66(H66A,H66B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C6(H6), C8(H8), C11(H11), C12(H12), C13(H13),
 C14(H14), C15(H15), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C23(H23),
  C24(H24), C25(H25), C26(H26), C27(H27), C30(H30), C31(H31), C32(H32),
 C33(H33), C34(H34), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C42(H42),
  C43(H43), C44(H44), C45(H45), C46(H46), C48(H48), C49(H49), C50(H50),
 C51(H51), C52(H52), C55(H55), C56(H56), C57(H57), C58(H58), C59(H59), C61(H61),
  C62(H62), C63(H63), C64(H64), C65(H65)
;
_olex2_submission_special_instructions 'No special instructions were received'