Stepwise Formation of Heterobimetallic Macrocycles Synthesized via the Weak-Link Approach
Adam H. Eisenberg; Maxim V. Ovchinnikov; Chad A. Mirkin; Journal of the American Chemical Society 125 (2003) 2836–2837; doi:10.1021/ja027936n

data_4113525
_publ_section_title
;
 Stepwise Formation of Heterobimetallic Macrocycles Synthesized via the
 Weak-Link Approach
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2836
_journal_page_last               2837
_journal_paper_doi               10.1021/ja027936n
_journal_volume                  125
_journal_year                    2003
_chemical_formula_moiety         'C34 H32 O P2 S '
_chemical_formula_sum            'C34 H32 O P2 S'
_chemical_formula_weight         550.63
_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'
_cell_angle_alpha                64.339(3)
_cell_angle_beta                 81.984(3)
_cell_angle_gamma                86.122(4)
_cell_formula_units_Z            2
_cell_length_a                   5.6168(11)
_cell_length_b                   16.076(3)
_cell_length_c                   17.651(4)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    153.2
_cell_measurement_theta_max      0.0
_cell_measurement_theta_min      0.0
_cell_volume                     1422.5(5)
_computing_cell_refinement       'Bruker SAINT-1000 Diffractometer Control'
_computing_data_collection       'Bruker SMART-1000 Diffractometer Control'
_computing_data_reduction        'Bruker SAINT-1000 Diffractometer Control'
_computing_publication_material
;
teXsan for Windows version 1.06 (MSC, 1997-1999)
;
_computing_structure_refinement
;
teXsan for Windows version 1.06 (MSC, 1997-1999)
;
_computing_structure_solution
;
SHELX97 (Sheldrick, 1997)
;
_diffrn_ambient_temperature      153.2
_diffrn_measurement_device       'Bruker SMART-1000 CCD'
_diffrn_measurement_method       \w
_diffrn_orient_matrix_UB_11      0.00000
_diffrn_orient_matrix_UB_12      0.00000
_diffrn_orient_matrix_UB_13      0.00000
_diffrn_orient_matrix_UB_21      0.00000
_diffrn_orient_matrix_UB_22      0.00000
_diffrn_orient_matrix_UB_23      0.00000
_diffrn_orient_matrix_UB_31      0.00000
_diffrn_orient_matrix_UB_32      0.00000
_diffrn_orient_matrix_UB_33      0.00000
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.07155
_diffrn_reflns_av_sigmaI/netI    0.117
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            13144
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.29
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.252
_exptl_absorpt_correction_T_max  0.98613
_exptl_absorpt_correction_T_min  0.95232
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_description       block
_exptl_crystal_F_000             580.00
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.09
_refine_diff_density_min         -0.75
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.660
_refine_ls_goodness_of_fit_ref   2.240
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     343
_refine_ls_number_reflns         3023
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1424
_refine_ls_R_factor_gt           0.064
_refine_ls_shift/su_max          0.0100
_refine_ls_shift/su_mean         0.0011
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo)]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.1400
_refine_ls_wR_factor_ref         0.059
_reflns_number_gt                3023
_reflns_number_total             6604
_reflns_threshold_expression     I>3.00\s(I)
_cod_data_source_file            ja027936nsi20030121_083210.cif
_cod_data_source_block           '_Template_texray.inf'
_cod_original_formula_sum        'C34 H32 O P2 S '
_cod_database_code               4113525