Calix[4]arene-fused phospholes
Elaieb, Fethi; Sémeril, David; Matt, Dominique; Pfeffer, Michel; Bouit, Pierre-Antoine; Hissler, Muriel; Gourlaouen, Christophe; Harrowfield, Jack; Dalton Trans.  (2017) –; doi:10.1039/C7DT01899A

data_7043532
_publ_section_title
;
 Calix[4]arene-fused phospholes
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01899A
_journal_year                    2017
_chemical_formula_moiety         'C62 H63 Cl N O4 P Pd'
_chemical_formula_sum            'C62 H63 Cl N O4 P Pd'
_chemical_formula_weight         1058.95
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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-2013
_audit_update_record
;
2017-04-21 deposited with the CCDC.
2017-07-06 downloaded from the CCDC.
;
_cell_angle_alpha                94.474(2)
_cell_angle_beta                 90.746(2)
_cell_angle_gamma                91.791(2)
_cell_formula_units_Z            4
_cell_length_a                   9.8908(7)
_cell_length_b                   19.6964(14)
_cell_length_c                   27.456(2)
_cell_measurement_reflns_used    9935
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.04
_cell_measurement_theta_min      2.26
_cell_volume                     5329.2(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  triumph
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0946
_diffrn_reflns_av_unetI/netI     0.1328
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            71514
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.097
_diffrn_reflns_theta_min         1.228
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.477
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6086
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_description       prism
_exptl_crystal_F_000             2208
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.140
_refine_diff_density_max         2.058
_refine_diff_density_min         -2.031
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1298
_refine_ls_number_reflns         25707
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1495
_refine_ls_R_factor_gt           0.0782
_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^)+(0.0537P)^2^+15.5771P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1526
_refine_ls_wR_factor_ref         0.1776
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15303
_reflns_number_total             25707
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01899a2.cif
_cod_data_source_block           dmfe170330
_cod_database_code               7043532
_shelx_estimated_absorpt_t_min   0.890
_shelx_estimated_absorpt_t_max   0.936
_shelxl_version_number           2013-4
_shelx_res_checksum              6855