Metallic Macrocycle with a 1,3-Alternate Calix[4]arene Phosphorus Ligand
Sanghoon Kim; Jong Seung Kim; Ok Jae Shon; Shim Sung Lee; Ki-Min Park; Sang Ook Kang; Jaejung Ko; Inorganic Chemistry 43 (2004) 2906–2913; doi:10.1021/ic030221g

data_4310890
_publ_section_title
;
 Metallic Macrocycle with a 1,3-Alternate Calix[4]arene Phosphorus Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2906
_journal_page_last               2913
_journal_paper_doi               10.1021/ic030221g
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C62 H62 O4 P2'
_chemical_formula_weight         933.06
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   constr
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 120.196(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.0299(18)
_cell_length_b                   16.2113(15)
_cell_length_c                   18.4857(16)
_cell_measurement_temperature    298(2)
_cell_volume                     5188.0(8)
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        'SHELXTL (Siemens, 1996)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    SHELXTL
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_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  0.0645
_diffrn_reflns_av_sigmaI/netI    0.0747
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16900
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    0.131
_exptl_crystal_density_diffrn    1.195
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1984
_refine_diff_density_max         0.384
_refine_diff_density_min         -0.181
_refine_diff_density_rms         0.036
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         6256
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.1724
_refine_ls_R_factor_gt           0.0623
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0853P)^2^+0.3655P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1478
_refine_ls_wR_factor_ref         0.1921
_reflns_number_gt                2526
_reflns_number_total             6256
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic030221g_1.cif
_cod_data_source_block           kjj21
_cod_database_code               4310890