Synthesis of planar macrocyclic tetradentate phosphine-Mo complexes.
Wang, Xinchao; Liao, Qian; Dalton transactions (Cambridge, England : 2003) 54 (2025) 8769–8772; doi:10.1039/d5dt00984g

data_7718691
_publ_section_title
;
 Synthesis of planar macrocyclic tetradentate phosphine-Mo complexes.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8769
_journal_page_last               8772
_journal_paper_doi               10.1039/d5dt00984g
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C18 H37 Mo O2 P4, F6 P'
_chemical_formula_sum            'C18 H37 F6 Mo O2 P5'
_chemical_formula_weight         650.26
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive
_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   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2025-03-24 deposited with the CCDC.	2025-05-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.768(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2715(6)
_cell_length_b                   9.0595(4)
_cell_length_c                   25.2626(14)
_cell_measurement_reflns_used    9070
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.55
_cell_measurement_theta_min      3.35
_cell_volume                     2515.9(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0589
_diffrn_reflns_av_unetI/netI     0.0622
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            23192
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.557
_diffrn_reflns_theta_min         2.248
_exptl_absorpt_coefficient_mu    0.899
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5794
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.717
_exptl_crystal_description       block
_exptl_crystal_F_000             1328
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: n-hexane and dichloromethane'
_exptl_crystal_size_max          0.472
_exptl_crystal_size_mid          0.137
_exptl_crystal_size_min          0.076
_refine_diff_density_max         0.927
_refine_diff_density_min         -0.879
_refine_diff_density_rms         0.187
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         7183
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0453
_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^)+4.9804P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1005
_refine_ls_wR_factor_ref         0.1069
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6108
_reflns_number_total             7183
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00984g2.cif
_cod_data_source_block           '[(HPPPPH)Mo(O)(OMe)][PF6]'
_cod_depositor_comments
'Adding full bibliography for 7718689--7718693.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7718691
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.676
_shelx_estimated_absorpt_t_max   0.935
_shelx_res_checksum              29764
_shelx_hkl_checksum              7964