Formation of paramagnetic metallacyclobutadienes by reaction of diaminoacetylenes with molybdenum alkylidyne complexes.
Àrias, Òscar; Brandhorst, Kai; Baabe, Dirk; Freytag, Matthias; Jones, Peter G.; Tamm, Matthias; Dalton transactions (Cambridge, England : 2003) 46 (2017) 4737–4748; doi:10.1039/c7dt00305f

data_7042387
_publ_section_title
;
 Formation of paramagnetic metallacyclobutadienes by reaction of
 diaminoacetylenes with molybdenum alkylidyne complexes.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4737
_journal_page_last               4748
_journal_paper_doi               10.1039/c7dt00305f
_journal_volume                  46
_journal_year                    2017
_chemical_formula_sum            'C32 H40 F18 Mo N2 O3'
_chemical_formula_weight         938.60
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-08-16 deposited with the CCDC.
2017-03-08 downloaded from the CCDC.
;
_cell_angle_alpha                88.000(2)
_cell_angle_beta                 73.097(3)
_cell_angle_gamma                82.987(3)
_cell_formula_units_Z            2
_cell_length_a                   12.5635(5)
_cell_length_b                   12.6072(4)
_cell_length_c                   12.7731(4)
_cell_measurement_reflns_used    54017
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.1850
_cell_measurement_theta_min      3.5060
_cell_volume                     1921.25(12)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Bruker XP'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3543
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur, Atlas, Nova'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0556
_diffrn_reflns_av_sigmaI/netI    0.0192
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            119615
_diffrn_reflns_theta_full        75.00
_diffrn_reflns_theta_max         76.32
_diffrn_reflns_theta_min         3.53
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    3.927
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.14737
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_exptl_crystal_colour            'brown-orange dichroic'
_exptl_crystal_density_diffrn    1.622
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             948
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.793
_refine_diff_density_min         -0.876
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     555
_refine_ls_number_reflns         8009
_refine_ls_number_restraints     98
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0485P)^2^+1.5345P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0818
_refine_ls_wR_factor_ref         0.0833
_reflns_number_gt                7588
_reflns_number_total             8009
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7dt00305f3.cif
_cod_data_source_block           oscar31
_cod_depositor_comments
'Adding full bibliography for 7042387--7042388.cif.'
_cod_original_cell_volume        1921.25(11)
_cod_database_code               7042387