Molybdenum(0) tricarbonyl and tetracarbonyl complexes with a cationic pyrazolylpyridine ligand: synthesis, crystal structures and catalytic performance in olefin epoxidation
Nogueira, Lucie S.; Neves, Patrícia; Gomes, Ana C.; Lavrador, Pedro; Cunha-Silva, Luís; Valente, Anabela A.; Gonçalves, Isabel S.; Pillinger, Martyn; RSC Advances 8 (2018) 16294–; doi:10.1039/C8RA01687A

data_7230575
_publ_section_title
;
 Molybdenum(0) tricarbonyl and tetracarbonyl complexes with a cationic
 pyrazolylpyridine ligand: synthesis, crystal structures and catalytic
 performance in olefin epoxidation
;
_journal_issue                   29
_journal_name_full               'RSC Advances'
_journal_page_first              16294
_journal_paper_doi               10.1039/C8RA01687A
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety         'C18 H21 Mo N4 O4, C2 H3 N, Br'
_chemical_formula_sum            'C20 H24 Br Mo N5 O4'
_chemical_formula_weight         574.29
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             '18 December 2016'
_audit_creation_method           'SHELXL-2014/7 and enCIFer'
_audit_update_record
;
2016-12-20 deposited with the CCDC.
2018-04-24 downloaded from the CCDC.
;
_cell_angle_alpha                87.812(7)
_cell_angle_beta                 88.701(8)
_cell_angle_gamma                87.216(7)
_cell_formula_units_Z            2
_cell_length_a                   7.5420(12)
_cell_length_b                   8.9322(12)
_cell_length_c                   17.705(3)
_cell_measurement_reflns_used    9235
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.78
_cell_measurement_theta_min      2.35
_cell_volume                     1190.2(3)
_computing_cell_refinement       'SAINT (Bruker AXS Inc., 2012)'
_computing_data_collection       'APEX2 (Bruker AXS Inc., 2012)'
_computing_data_reduction        'SAINT (Bruker AXS Inc., 2012)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2009)'
_computing_publication_material  'SHELXTL (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker X8 Kappa CCD APEX II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            40010
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         3.688
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.264
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.834
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
'SADABS V2012/1 (Bruker AXS Inc.)' 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_description       prism
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.776
_refine_diff_density_min         -0.550
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         4843
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0241
_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^)+(0.0225P)^2^+0.8444P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0529
_refine_ls_wR_factor_ref         0.0555
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4220
_reflns_number_total             4843
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ra01687a2.cif
_cod_data_source_block           lcs16002-comp1
_cod_database_code               7230575
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.840
_shelx_estimated_absorpt_t_max   0.935
_shelx_res_checksum              89019