Phenylphosphinacalix[3]trifuran: synthesis, coordination and application in the Suzuki-Miyaura cross-coupling reaction in water
Sun, Yue; Yan, Meng-Qi; Liu, Yan; Lian, Ze-Yu; Meng, Tong; chen, Jian; Liu, Shenghua; Yu, Guang-Ao; RSC Adv.  (2015) –; doi:10.1039/C5RA11778J

data_7221774
_publ_section_title
;
 Phenylphosphinacalix[3]trifuran: synthesis, coordination and application
 in the Suzuki-Miyaura cross-coupling reaction in water
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA11778J
_journal_year                    2015
_chemical_formula_sum            'C60.5 H42.5 Cl1.5 O6 P6 Se6'
_chemical_formula_weight         1578.20
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2012-01-13 deposited with the CCDC.
2015-08-10 downloaded from the CCDC.
;
_cell_angle_alpha                83.949(3)
_cell_angle_beta                 84.534(3)
_cell_angle_gamma                77.702(3)
_cell_formula_units_Z            2
_cell_length_a                   11.165(2)
_cell_length_b                   12.927(3)
_cell_length_c                   21.775(4)
_cell_measurement_reflns_used    7334
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.25
_cell_measurement_theta_min      2.16
_cell_volume                     3045.0(11)
_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-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_sigmaI/netI    0.0666
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            20584
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    3.879
_exptl_absorpt_correction_T_max  0.6532
_exptl_absorpt_correction_T_min  0.5657
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick,1997'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1546
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.462
_refine_diff_density_min         -3.006
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     733
_refine_ls_number_reflns         10542
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.1081
_refine_ls_R_factor_gt           0.0810
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0880P)^2^+36.2766P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2066
_refine_ls_wR_factor_ref         0.2184
_reflns_number_gt                8044
_reflns_number_total             10542
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ra11778j2.cif
_cod_data_source_block           mo_111127a_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 
;
_cod_original_cell_volume        3044.9(10)
_cod_original_formula_sum        'C60.50 H42.50 Cl1.50 O6 P6 Se6'
_cod_database_code               7221774