Mo(0) carbonyl complexes bearing the bis(3,5-dimethylpyrazole) ligand: catalysis of the regioselective [2 + 2 + 2] cycloaddition of terminal alkynes to synthesize 1,3,5-isomers.
Mondal, Palash; Dutta, Poulami; Mani, Ganesan; Dalton transactions (Cambridge, England : 2003) 54 (2025) 2654–2663; doi:10.1039/d4dt02725f

data_7717708
_publ_section_title
;
 Mo(0) carbonyl complexes bearing the bis(3,5-dimethylpyrazole) ligand:
 catalysis of the regioselective [2 + 2 + 2] cycloaddition of terminal
 alkynes to synthesize 1,3,5-isomers.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2654
_journal_page_last               2663
_journal_paper_doi               10.1039/d4dt02725f
_journal_volume                  54
_journal_year                    2025
_chemical_formula_sum            'C32 H40 Cl4 Mo2 N8 O8'
_chemical_formula_weight         998.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-09-25 deposited with the CCDC.	2024-12-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.7300(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.6388(7)
_cell_length_b                   13.4796(5)
_cell_length_c                   16.9256(6)
_cell_measurement_reflns_used    71428
_cell_measurement_temperature    102(2)
_cell_measurement_theta_max      24.997
_cell_measurement_theta_min      1.893
_cell_volume                     4072.5(3)
_computing_molecular_graphics    ORTEP
_computing_publication_material  ciftab
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      102(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'D8 QUEST'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0616
_diffrn_reflns_av_unetI/netI     0.0267
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            71428
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         1.893
_diffrn_source                   'Fine focused sealed tube'
_exptl_absorpt_coefficient_mu    0.935
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            brownish-yellow
_exptl_crystal_density_diffrn    1.628
_exptl_crystal_description       prism
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.067
_exptl_crystal_size_min          0.026
_exptl_transmission_factor_max   0.7455
_exptl_transmission_factor_min   0.6872
_refine_diff_density_max         1.835
_refine_diff_density_min         -0.951
_refine_diff_density_rms         0.091
_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     523
_refine_ls_number_reflns         7155
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0374
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0456P)^2^+10.6387P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0933
_refine_ls_wR_factor_ref         0.0971
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6242
_reflns_number_total             7155
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02725f2.cif
_cod_data_source_block           binuclearMo
_cod_depositor_comments
'Adding full bibliography for 7717708--7717709.cif.'
_cod_original_cell_volume        4072.4(3)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7717708
_shelx_shelxl_version_number     2019/3
_shelx_res_checksum              95975