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_7042388
_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            'C36 H44 F18 Mo N2 O3'
_chemical_formula_weight         990.67
_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                101.495(5)
_cell_angle_beta                 110.382(6)
_cell_angle_gamma                95.857(4)
_cell_formula_units_Z            2
_cell_length_a                   11.2300(6)
_cell_length_b                   12.6831(6)
_cell_length_c                   15.8296(10)
_cell_measurement_reflns_used    36004
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.6330
_cell_measurement_theta_min      3.6320
_cell_volume                     2034.7(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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 0.998
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur, Atlas, Nova'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Nova (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0810
_diffrn_reflns_av_sigmaI/netI    0.0307
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            92647
_diffrn_reflns_theta_full        75.00
_diffrn_reflns_theta_max         76.23
_diffrn_reflns_theta_min         3.62
_exptl_absorpt_coefficient_mu    3.744
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.03587
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1004
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.777
_refine_diff_density_min         -1.421
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     569
_refine_ls_number_reflns         8408
_refine_ls_number_restraints     112
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0492
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0763P)^2^+3.2856P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1255
_refine_ls_wR_factor_ref         0.1279
_reflns_number_gt                7883
_reflns_number_total             8408
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7dt00305f3.cif
_cod_data_source_block           oscar07
_cod_depositor_comments
'Adding full bibliography for 7042387--7042388.cif.'
_cod_original_cell_volume        2034.68(19)
_cod_database_code               7042388