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_7717775
_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         'C41 H31 F6 Mo N5 O2 P2'
_chemical_formula_sum            'C41 H31 F6 Mo N5 O2 P2'
_chemical_formula_weight         897.59
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-11-15 deposited with the CCDC.	2025-01-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.9270(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8694(2)
_cell_length_b                   17.5030(2)
_cell_length_c                   16.2883(2)
_cell_measurement_reflns_used    38057
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      79.5230
_cell_measurement_theta_min      3.7410
_cell_volume                     3837.85(9)
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_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  0.0484
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            64919
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.074
_diffrn_reflns_theta_min         3.766
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.224
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81731
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.120a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.710
_refine_diff_density_min         -0.867
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     516
_refine_ls_number_reflns         7276
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0349
_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^)+(0.0513P)^2^+4.1422P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0908
_refine_ls_wR_factor_ref         0.0925
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6704
_reflns_number_total             7276
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03264k2.cif
_cod_data_source_block           20230510AEN
_cod_depositor_comments
'Adding full bibliography for 7717773--7717778.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7717775
_shelx_shelxl_version_number     2019/3
_shelx_res_checksum              90790