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_7718689
_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         'C17 H32 P4,  I2'
_chemical_formula_sum            'C17 H32 I2 P4'
_chemical_formula_weight         614.10
_chemical_properties_physical    Light-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 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
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_cell_angle_gamma                90
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_cell_length_c                   13.3724(5)
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_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      70.03
_cell_measurement_theta_min      3.71
_cell_volume                     2309.22(16)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0634
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            33796
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.048
_diffrn_reflns_theta_min         6.811
_exptl_absorpt_coefficient_mu    23.985
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.3640
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.766
_exptl_crystal_description       block
_exptl_crystal_F_000             1200
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol'
_exptl_crystal_size_max          0.261
_exptl_crystal_size_mid          0.126
_exptl_crystal_size_min          0.115
_refine_diff_density_max         1.142
_refine_diff_density_min         -0.835
_refine_diff_density_rms         0.128
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.048(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         4176
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0315
_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^)+(0.0633P)^2^+0.2834P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0795
_refine_ls_wR_factor_ref         0.0796
_reflns_Friedel_coverage         0.998
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                4162
_reflns_number_total             4176
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00984g2.cif
_cod_data_source_block           '[PP]I2'
_cod_depositor_comments
'Adding full bibliography for 7718689--7718693.cif.'
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               7718689
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.062
_shelx_estimated_absorpt_t_max   0.169
_shelx_res_checksum              42768
_shelx_hkl_checksum              8874