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_7717709
_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            'C20 H26 Mo N6 O4'
_chemical_formula_weight         510.41
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/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                 93.962(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.534(3)
_cell_length_b                   9.0364(8)
_cell_length_c                   18.5849(16)
_cell_measurement_reflns_used    5466
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.452
_cell_measurement_theta_min      2.365
_cell_volume                     4780.6(8)
_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      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_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  0.0450
_diffrn_reflns_av_unetI/netI     0.0225
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            49414
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.452
_diffrn_reflns_theta_min         2.365
_diffrn_source                   'Fine focused sealed tube'
_exptl_absorpt_coefficient_mu    0.585
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_description       needle
_exptl_crystal_F_000             2096
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.006
_exptl_transmission_factor_max   0.7455
_exptl_transmission_factor_min   0.6605
_refine_diff_density_max         0.237
_refine_diff_density_min         -0.449
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         5463
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0248
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0309P)^2^+2.9705P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0650
_refine_ls_wR_factor_ref         0.0674
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4854
_reflns_number_total             5463
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02725f2.cif
_cod_data_source_block           mononuclearMo
_cod_depositor_comments
'Adding full bibliography for 7717708--7717709.cif.'
_cod_original_cell_volume        4780.5(7)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7717709
_shelx_shelxl_version_number     2019/3
_shelx_res_checksum              94017