Modular synthesis of triphenylphosphine-derived cage ligands for rhodium-catalyzed hydroformylation applications.
Wang, Wenlong; Li, Cunyao; Wang, Wenhao; Qiu, Yuqin; Liu, Hongguang; Lu, Jinlong; Zhan, Yizhou; Yan, Li; Ding, Yunjie; Dalton transactions (Cambridge, England : 2003) 54 (2024) 207–214; doi:10.1039/d4dt02627f

data_7717450
_publ_section_title
;
 Modular synthesis of triphenylphosphine-derived cage ligands for
 rhodium-catalyzed hydroformylation applications.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              207
_journal_page_last               214
_journal_paper_doi               10.1039/d4dt02627f
_journal_volume                  54
_journal_year                    2024
_chemical_formula_moiety         '0.04(C60 H50 F12 N6 P2), 0.04(C H2 Cl2)'
_chemical_formula_sum            'C H Cl0.01 F N P'
_chemical_formula_weight         77.23
_space_group_crystal_system      hexagonal
_space_group_IT_number           179
_space_group_name_Hall           'P 65 2 (0 0 1)'
_space_group_name_H-M_alt        'P 65 2 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-11-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-03-15 deposited with the CCDC.	2024-10-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            155
_cell_length_a                   23.8636(12)
_cell_length_b                   23.8636(12)
_cell_length_c                   22.2433(10)
_cell_measurement_reflns_used    9946
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      23.32
_cell_measurement_theta_min      2.50
_cell_volume                     10969.9(9)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      250.01
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_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  0.0529
_diffrn_reflns_av_unetI/netI     0.0574
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            37707
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.572
_diffrn_reflns_theta_min         2.173
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.703
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6674
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1311 before and 0.0431 after correction.
The Ratio of minimum to maximum transmission is 0.8951.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.812
_exptl_crystal_F_000             5907
_refine_diff_density_max         0.821
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details
;
 Flack x determined using 1105 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.07(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         8447
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1934
_refine_ls_R_factor_gt           0.0992
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1826P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2522
_refine_ls_wR_factor_ref         0.3238
_reflns_Friedel_coverage         0.760
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                3606
_reflns_number_total             8447
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02627f2.cif
_cod_data_source_block           mo_20191127_3_0m_a
_cod_depositor_comments
'Adding full bibliography for 7717449--7717451.cif.'
_cod_original_cell_volume        10969.9(12)
_cod_database_code               7717450
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Others
 Fixed Sof: H00E(0.5) H00F(0.5)
3.a Ternary CH refined with riding coordinates:
 C009(H009), C011(H011), C012(H012)
3.b Secondary CH2 refined with riding coordinates:
 C00F(H00A,H00B), C00N(H00C,H00D), C00Z(H00E,H00F), C013(H01A,H01B), C014(H01C,
 H01D), C015(H01E,H01F), C016(H01G,H01H)
3.c Aromatic/amide H refined with riding coordinates:
 C007(H007), C00O(H00O), C00Q(H00Q), C00S(H00S), C00T(H00T), C00U(H00U),
 C00W(H00W), C00X(H00X), N00Y(H00Y), C010(H010)
;
_shelx_res_checksum              59144
_shelx_hkl_checksum              79789
_olex2_submission_special_instructions 'No special instructions were received'