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_7027709
_publ_section_title
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 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         'C146 H170 Cl16 O9 P4 Pt2'
_chemical_formula_sum            'C146 H170 Cl16 O9 P4 Pt2'
_chemical_formula_weight         3150.30
_chemical_name_systematic        ' ?'
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.571(1)
_cell_length_b                   22.5546(3)
_cell_length_c                   26.4894(3)
_cell_measurement_reflns_used    50394
_cell_measurement_temperature    173
_cell_measurement_theta_max      32.4
_cell_measurement_theta_min      1.4
_cell_volume                     7510.6(6)
_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
;
144 frames,109 sec/frame, delta phi = 1.3 deg. Each frame measured 2 times.
Detector to crystal distance 32 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  0.063
_diffrn_reflns_av_sigmaI/netI    0.333
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            50394
_diffrn_reflns_theta_max         32.39
_diffrn_reflns_theta_min         2.5
_diffrn_source                   xray_tube
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.241
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.39
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             3212
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.416
_refine_diff_density_min         -0.190
_refine_ls_abs_structure_details 'Flack H D  (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(1)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   5.859
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     824
_refine_ls_number_reflns         9230
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.068
_refine_ls_R_factor_gt           0.050
_refine_ls_shift/esd_mean        0.002
_refine_ls_shift/su_max          0.030
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 4Fo^2^/(\s^2^(Fo^2^) + 0.0064 Fo^4^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.371
_refine_ls_wR_factor_ref         0.068
_reflns_number_gt                9230
_reflns_number_total             13123
_reflns_threshold_expression     >3.0\s(I)
_cod_data_source_file            905814asup1.cif
_cod_data_source_block           st329
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '4Fo^2^/(\s^2^(Fo^2^) + 0.0064
Fo^4^)' 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^) + 0.0064 Fo^4^)'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_cell_volume        7510.6(8)
_cod_original_sg_symbol_Hall     ' P 2ac 2ab'
_cod_database_code               7027709