Dual nucleophilic substitution at a W(ii) η(2)-coordinated diiodo acetylene leading to an amidinium carbyne complex.
Helmdach, Kai; Rüger, Julia; Villinger, Alexander; Seidel, Wolfram W.; Chemical communications (Cambridge, England) 52 (2016) 2616–2619; doi:10.1039/c5cc10397e

data_7118243
_publ_section_title
;
 Dual nucleophilic substitution at a W(ii) \h(2)-coordinated diiodo
 acetylene leading to an amidinium carbyne complex.
;
_journal_issue                   12
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2616
_journal_page_last               2619
_journal_paper_doi               10.1039/c5cc10397e
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C25 H32 B I2 N8 O W +, F6 P - '
_chemical_formula_sum            'C25 H32 B F6 I2 N8 O P W'
_chemical_formula_weight         1054.01
_chemical_name_systematic
Carbonyl-diiodacetylene-dimethylaminopyridine-hydridotris(3,5-dimethylpyrazolylborato)tungsten(II)-hexafluorophosphate
_chemical_properties_physical    'Air-sensitive, Light-sensitive'
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-09-30 deposited with the CCDC.
2016-01-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.772(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.3520(2)
_cell_length_b                   22.5729(6)
_cell_length_c                   18.2914(5)
_cell_measurement_reflns_used    2078
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      21.79
_cell_measurement_theta_min      2.53
_cell_volume                     3387.69(15)
_computing_cell_refinement       'Bruker Apex V7.51A'
_computing_data_collection       'Bruker Apex V7.51A'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  SHELXL-2013
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker-Nonius Apex X8-CCD-diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1337
_diffrn_reflns_av_unetI/netI     0.1641
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            44292
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.999
_diffrn_reflns_theta_min         2.641
_exptl_absorpt_coefficient_mu    5.347
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6043
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.067
_exptl_crystal_description       needle
_exptl_crystal_F_000             2000
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane/n-pentane'
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.010
_refine_diff_density_max         2.264
_refine_diff_density_min         -1.670
_refine_diff_density_rms         0.253
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         8987
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.1608
_refine_ls_R_factor_gt           0.0635
_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^)+(0.0393P)^2^+14.2225P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1022
_refine_ls_wR_factor_ref         0.1327
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4646
_reflns_number_total             8987
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc10397e2.cif
_cod_data_source_block           is_kh066b
_cod_depositor_comments
'Adding full bibliography for 7118243--7118244.cif.'
_cod_database_code               7118243
_shelx_estimated_absorpt_t_min   0.414
_shelx_estimated_absorpt_t_max   0.948
_shelxl_version_number           2013-4
_shelx_res_checksum              47132