Facile self-assembly of the first diphosphametacyclophane
Amy J. Saunders; Ian R. Crossley; Martyn P. Coles; S. Mark Roe; Chem.Commun. 48 (2012) 5766–; doi:10.1039/c2cc32247a

data_7107787
_publ_section_title
;
 Facile self-assembly of the first diphosphametacyclophane
;
_journal_name_full               Chem.Commun.
_journal_page_first              5766
_journal_paper_doi               10.1039/c2cc32247a
_journal_volume                  48
_journal_year                    2012
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C36 H28 Cl2 O8 P4 Pt, 2(C4 H8 O)'
_chemical_formula_sum            'C44 H44 Cl2 O10 P4 Pt'
_chemical_formula_weight         1122.65
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2011-06-29T09:26:14-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                87.512(3)
_cell_angle_beta                 69.834(3)
_cell_angle_gamma                64.064(3)
_cell_formula_units_Z            1
_cell_length_a                   10.4564(4)
_cell_length_b                   11.3437(6)
_cell_length_c                   11.5627(7)
_cell_measurement_reflns_used    34327
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.733
_cell_measurement_theta_min      3.395
_cell_measurement_wavelength     0.71073
_cell_volume                     1148.36(11)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.105302
_diffrn_orient_matrix_UB_12      0.7833E-2
_diffrn_orient_matrix_UB_13      0.255312E-1
_diffrn_orient_matrix_UB_21      0.386815E-1
_diffrn_orient_matrix_UB_22      -0.763859E-1
_diffrn_orient_matrix_UB_23      -0.636761E-1
_diffrn_orient_matrix_UB_31      0.208948E-1
_diffrn_orient_matrix_UB_32      -0.622199E-1
_diffrn_orient_matrix_UB_33      0.626222E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15427
_diffrn_reflns_theta_full        26.79
_diffrn_reflns_theta_max         26.79
_diffrn_reflns_theta_min         3.49
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    3.366
_exptl_absorpt_correction_T_max  0.3095
_exptl_absorpt_correction_T_min  0.2635
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.623
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Rhombohedral
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.621
_refine_diff_density_min         -1.468
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         4843
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0261
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0409P)^2^+0.3959P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0653
_refine_ls_wR_factor_ref         0.0656
_reflns_number_gt                4812
_reflns_number_total             4843
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc32247a.txt
_cod_data_source_block           jun711
_cod_original_cell_volume        1148.36(10)
_cod_database_code               7107787