Co-ordination chemistry of macrocyclic compounds with dangling phosphines. Unusual NMR shifts in metallo-calix[4]arenes †
Dieleman, Cedric B.; Marsol, Claire; Matt, Dominique; Kyritsakas, Nathalie; Harriman, Anthony; Kintzinger, Jean-Pierre; Journal of the Chemical Society, Dalton Transactions  (1999) 4139–; doi:10.1039/a905814a

data_7027708
_publ_section_title
;
 Co-ordination chemistry of macrocyclic compounds with dangling
 phosphines. Unusual NMR shifts in metallo-calix[4]arenes&#x200A;&#x2020;
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_journal_issue                   23
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4139
_journal_paper_doi               10.1039/a905814a
_journal_year                    1999
_chemical_formula_moiety         'C144 H166 O13 P4'
_chemical_formula_sum            'C144 H166 O13 P4'
_chemical_formula_weight         2228.82
_chemical_name_systematic        ' ?'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                102.912(9)
_cell_angle_beta                 106.361(9)
_cell_angle_gamma                103.676(9)
_cell_formula_units_Z            1
_cell_length_a                   14.9993(8)
_cell_length_b                   15.351(1)
_cell_length_c                   15.4699(9)
_cell_measurement_reflns_used    22148
_cell_measurement_temperature    173
_cell_measurement_theta_max      26.4
_cell_measurement_theta_min      1.4
_cell_volume                     3156.1(5)
_computing_publication_material  CIFGEN_IN_OpenMoleN_(_1997)
_computing_structure_refinement  LSFM_OpenMoleN_(_1997)
_computing_structure_solution    Direct_methods_(SIR,_Burla_et_al.,_1989)
_diffrn_ambient_temperature      173
_diffrn_measurement_details
;
180 frames, 50 sec/frame, delta phi = 1.0 deg. Each frame measured 2 times.
Detector to crystal distance 25 mm.
;
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\p scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.075
_diffrn_reflns_av_sigmaI/netI    0.333
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22148
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         2.5
_diffrn_source                   xray_tube
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.116
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.17
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             1194
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.038
_refine_diff_density_min         -0.121
_refine_ls_abs_structure_details ' ?'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   2.047
_refine_ls_goodness_of_fit_ref   1.225
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     712
_refine_ls_number_reflns         5805
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.177
_refine_ls_R_factor_gt           0.085
_refine_ls_shift/esd_mean        0.001
_refine_ls_shift/su_max          0.036
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 4Fo^2^/(\s^2^(Fo^2^)+0.0016 Fo^4^)+4.0'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.181
_refine_ls_wR_factor_ref         0.109
_reflns_number_gt                5805
_reflns_number_total             11952
_reflns_threshold_expression     >3.0\s(I)
_cod_data_source_file            905814asup1.cif
_cod_data_source_block           st165
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '4Fo^2^/(\s^2^(Fo^2^)+0.0016
Fo^4^)+4.0' was changed to 'calc'. New tag
'_refine_ls_weighting_details' was created. The value of the new tag
was set to 'w = 4Fo^2^/(\s^2^(Fo^2^)+0.0016 Fo^4^)+4.0'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3156(1)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7027708