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_7230577
_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         'C14 H21 N4, Br'
_chemical_formula_sum            'C14 H21 Br N4'
_chemical_formula_weight         325.26
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                90
_cell_angle_beta                 94.711(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.0727(4)
_cell_length_b                   7.6409(3)
_cell_length_c                   22.0574(10)
_cell_measurement_reflns_used    9865
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.95
_cell_measurement_theta_min      2.82
_cell_volume                     1523.93(11)
_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 0.997
_diffrn_measured_fraction_theta_max 0.998
_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  0.0311
_diffrn_reflns_av_unetI/netI     0.0181
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            55072
_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         30.033
_diffrn_reflns_theta_min         3.659
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.691
_exptl_absorpt_correction_T_max  0.877
_exptl_absorpt_correction_T_min  0.675
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
'SADABS V2012/1 (Bruker AXS Inc.)' 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_description       prism
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.363
_refine_diff_density_min         -0.212
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         4440
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0232
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0258P)^2^+0.4929P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0511
_refine_ls_wR_factor_ref         0.0564
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3358
_reflns_number_total             4440
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ra01687a2.cif
_cod_data_source_block           ig0215-L1
_cod_database_code               7230577
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.629
_shelx_estimated_absorpt_t_max   0.877
_shelx_res_checksum              68681