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_7718692
_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         'C23 H43 Mo O3 P4, F6 P'
_chemical_formula_sum            'C23 H43 F6 Mo O3 P5'
_chemical_formula_weight         732.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_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                 107.8221(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.4237(7)
_cell_length_b                   9.6183(4)
_cell_length_c                   16.5169(6)
_cell_measurement_reflns_used    9646
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      63.39
_cell_measurement_theta_min      4.13
_cell_volume                     2937.66(19)
_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      170(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            26021
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         63.438
_diffrn_reflns_theta_min         2.445
_exptl_absorpt_coefficient_mu    4.532
_exptl_absorpt_correction_T_max  0.7523
_exptl_absorpt_correction_T_min  0.5326
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.656
_exptl_crystal_description       block
_exptl_crystal_F_000             1504
_exptl_crystal_recrystallization_method 'Vapour deposition'
_exptl_crystal_size_max          0.306
_exptl_crystal_size_mid          0.059
_exptl_crystal_size_min          0.057
_refine_diff_density_max         1.044
_refine_diff_density_min         -0.884
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.48(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         6980
_refine_ls_number_restraints     434
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0419
_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^)+(0.0260P)^2^+12.7117P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1085
_refine_ls_wR_factor_ref         0.1087
_reflns_Friedel_coverage         0.897
_reflns_Friedel_fraction_full    0.988
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                6939
_reflns_number_total             6980
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00984g2.cif
_cod_data_source_block           '[(PPCprPPOxt)Mo(O)(OMe)][PF6]'
_cod_depositor_comments
'Adding full bibliography for 7718689--7718693.cif.'
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               7718692
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.338
_shelx_estimated_absorpt_t_max   0.782
_shelx_res_checksum              46285
_shelx_hkl_checksum              7162