Synthesis and characterization of heptacoordinated molybdenum(II) complexes supported with 2,6-bis(pyrazol-3-yl)pyridine (bpp) ligands.
Estival, Arno; Blancarte, Luis E.; Pinto, Loïc; Pointis, Romane; Galas, Nathan; Sournia-Saquet, Alix; Vendier, Laure; Santillan, Rosa; Farfán, Norberto; Sortais, Jean-Baptiste; Grellier, Mary; Simonneau, Antoine; Dalton transactions (Cambridge, England : 2003) 54 (2025) 2860–2870; doi:10.1039/d4dt03264k

data_7717774
_publ_section_title
;
 Synthesis and characterization of heptacoordinated molybdenum(II)
 complexes supported with 2,6-bis(pyrazol-3-yl)pyridine (bpp) ligands.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2860
_journal_page_last               2870
_journal_paper_doi               10.1039/d4dt03264k
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C47 H51 Mo N5 O2 P2, 2(C F3 O3 S)'
_chemical_formula_sum            'C49 H51 F6 Mo N5 O8 P2 S2'
_chemical_formula_weight         1173.98
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_update_record
;
2024-12-13 deposited with the CCDC.	2025-01-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.741(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.4003(7)
_cell_length_b                   10.8477(5)
_cell_length_c                   23.6970(10)
_cell_measurement_reflns_used    22700
_cell_measurement_temperature    100
_cell_measurement_theta_max      74.63
_cell_measurement_theta_min      3.75
_cell_volume                     5729.3(4)
_computing_cell_refinement
; 
 CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)
;
_computing_data_collection       'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_computing_data_reduction
; 
 CrysAlisPro 1.171.42.102a (Rigaku OD, 2023) 
;
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.151
_diffrn_reflns_av_unetI/netI     0.106
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            81801
_diffrn_reflns_theta_full        74.390
_diffrn_reflns_theta_max         57.618
_diffrn_reflns_theta_min         3.749
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.702
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.46
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.42.102a (Rigaku OD, 2023) 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             2408
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.030
_refine_diff_density_max         2.27
_refine_diff_density_min         -0.67
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.3815
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         3909
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.1080
_refine_ls_R_factor_gt           0.1006
_refine_ls_shift/su_max          0.0001789
_refine_ls_shift/su_mean         0.0000139
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.20P)^2^ + 0.00P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3045
_refine_ls_wR_factor_gt          0.2946
_refine_ls_wR_factor_ref         0.3041
_reflns_limit_h_max              28
_reflns_limit_h_min              -28
_reflns_limit_k_max              13
_reflns_limit_k_min              0
_reflns_limit_l_max              30
_reflns_limit_l_min              0
_reflns_number_gt                3325
_reflns_number_total             5995
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_scale          0.462(3)
_cod_data_source_file            d4dt03264k2.cif
_cod_data_source_block           20240306eqNArno
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7717773--7717778.cif.
;
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_database_code               7717774
_oxford_refine_reflns_threshold_expression I>-3.0\s(I)
_refine_ls_r_factor_ref          0.1080
_reflns_number_all               3910
_platon_squeeze_void_probe_radius 1.20