Supramolecular bidentate phosphine ligand scaffolds from deconstructed Hamilton receptors.
Seidenkranz, Daniel T.; McGrath, Jacqueline M.; Zakharov, Lev N.; Pluth, Michael D.; Chemical communications (Cambridge, England) 53 (2017) 561–564; doi:10.1039/c6cc09198a

data_7119264
_publ_section_title
;
 Supramolecular bidentate phosphine ligand scaffolds from deconstructed
 Hamilton receptors.
;
_journal_issue                   3
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              561
_journal_page_last               564
_journal_paper_doi               10.1039/c6cc09198a
_journal_volume                  53
_journal_year                    2017
_chemical_formula_sum            'C34 H38 N3 O3 P'
_chemical_formula_weight         567.64
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-06-29 deposited with the CCDC.
2016-12-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.365(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.8728(3)
_cell_length_b                   9.3584(4)
_cell_length_c                   18.8092(6)
_cell_measurement_reflns_used    5023
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      69.21
_cell_measurement_theta_min      4.70
_cell_volume                     1561.38(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHEXLTL'
_computing_publication_material  'Bruker SHEXLTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.966
_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  0.0378
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            10353
_diffrn_reflns_point_group_measured_fraction_full 0.835
_diffrn_reflns_point_group_measured_fraction_max 0.814
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         69.469
_diffrn_reflns_theta_min         2.350
_diffrn_source                   'Incoatec I\mS'
_exptl_absorpt_coefficient_mu    1.075
_exptl_absorpt_correction_T_max  0.7532
_exptl_absorpt_correction_T_min  0.6764
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_description       prizm
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.464
_refine_diff_density_min         -0.222
_refine_diff_density_rms         0.043
_refine_ls_abs_structure_details
;
 Flack x determined using 1471 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.042(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     490
_refine_ls_number_reflns         4779
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0389
_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^)+(0.0543P)^2^+0.0922P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0985
_refine_ls_wR_factor_ref         0.1014
_reflns_Friedel_coverage         0.580
_reflns_Friedel_fraction_full    0.661
_reflns_Friedel_fraction_max     0.640
_reflns_number_gt                4406
_reflns_number_total             4779
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc09198a2.cif
_cod_data_source_block           cu_mplu29_0m
_cod_database_code               7119264
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.838
_shelx_estimated_absorpt_t_max   0.891
_shelx_res_checksum              65695
_shelx_hkl_checksum              83729