Carbyne‒Carbyne Coupling and H-Shifts in Reactions of the Unsaturated Methoxy- and Hydroxycarbyne Complexes [Mo2Cp2(μ-COR)(μ-CPh)(μ-PCy2)]+ with CO and Isocyanides
Alvarez, M. Angeles; García, M. Esther; Menéndez, Sonia; Ruiz, Miguel A.; Organometallics 34 (2015) 1681–; doi:10.1021/acs.organomet.5b00166

data_4087485
_publ_section_title
;
 Carbyne--Carbyne Coupling and H-Shifts in Reactions of the Unsaturated
 Methoxy- and Hydroxycarbyne Complexes [Mo2Cp2(\m-COR)(\m-CPh)(\m-PCy2)]+
 with CO and Isocyanides
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              1681
_journal_paper_doi               10.1021/acs.organomet.5b00166
_journal_volume                  34
_journal_year                    2015
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C44 H65 Mo2 N3 P, B F4 '
_chemical_formula_sum            'C44 H65 B F4 Mo2 N3 P'
_chemical_formula_weight         945.65
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_audit_creation_method           'WinGX routine CIF_UPDATE'
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_cell_angle_gamma                90
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_cell_length_b                   12.1958(12)
_cell_length_c                   19.7064(18)
_cell_measurement_reflns_used    1921
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_cell_measurement_theta_min      2.25
_cell_measurement_wavelength     0.71073
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_computing_cell_refinement       'BRUKER APEX'
_computing_data_collection       'BRUKER APEX'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'BRUKER APPEX-II CCD'
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_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0863
_diffrn_reflns_av_unetI/netI     0.0591
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            66917
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    0.659
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7509
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER Sadabs'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3920
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     499
_refine_ls_number_reflns         8637
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_gt           0.0493
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0816P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1177
_refine_ls_wR_factor_ref         0.1278
_reflns_number_gt                6432
_reflns_number_total             8637
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5b00166_si_002.cif
_cod_data_source_block           compound7a
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '_diffrn_radiation_monochromador' was replaced with
'_diffrn_radiation_monochromator' as specified in the replacement
file
'/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/lists/replacement-tags.lst'.

Automatic conversion script
Id: cif_correct_tags 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        8773.7(14)
_cod_database_code               4087485