Flexible Building Blocks for Transition Metal Early−Late Chemistry. Synthesis of Heterobimetallic Tetranuclear Metallomacrocycles
Álvarez-Vergara, M. Carmen; Casado, Miguel A.; Martín, M. Luisa; Lahoz, Fernando J.; Oro, Luis A.; Pérez-Torrente, Jesús J.; Organometallics 24 (2005) 5929–; doi:10.1021/om050644l

data_4076143
_publ_section_title
;
 Flexible Building Blocks for Transition Metal Early&#x2212;Late
 Chemistry. Synthesis of Heterobimetallic Tetranuclear Metallomacrocycles
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              5929
_journal_paper_doi               10.1021/om050644l
_journal_volume                  24
_journal_year                    2005
_chemical_formula_moiety         'C88 H92 Ir2 O4 P4 Zr2, 4(C H2 Cl2), 2(B F4)'
_chemical_formula_sum            'C92 H100 B2 Cl8 F8 Ir2 O4 P4 Zr2'
_chemical_formula_weight         2417.66
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.8530(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.4325(10)
_cell_length_b                   15.4098(10)
_cell_length_c                   19.5915(13)
_cell_measurement_reflns_used    5624
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.15
_cell_measurement_theta_min      2.47
_cell_volume                     4615.4(5)
_computing_cell_refinement       'SAINT+ v. 6.01 (Bruker AXS, 2000)'
_computing_data_collection       'SMART v. 5.611 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+ v. 6.01 (Bruker AXS, 2000)'
_computing_molecular_graphics    'XP program, SHELXTL v6.12, Bruker2000'
_computing_publication_material  'XCIF program, SHELXTLv6.12, BrukerAXS'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.907
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_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  0.0261
_diffrn_reflns_av_sigmaI/netI    0.0452
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            29387
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.43
_diffrn_reflns_theta_min         1.58
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    3.461
_exptl_absorpt_correction_T_max  0.4197
_exptl_absorpt_correction_T_min  0.3488
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS: Area-Detector Absorption Correction. (1996)  Bruker-AXS 
 within SAINT+ package, v. 6.01.                    
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.740
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             2392
_exptl_crystal_size_max          0.328
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.251
_refine_diff_density_max         4.219
_refine_diff_density_min         -1.293
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         10544
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0425
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0720P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1138
_refine_ls_wR_factor_ref         0.1178
_reflns_number_gt                8583
_reflns_number_total             10544
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om050644lsi20050728_053646.cif
_cod_data_source_block           compd7
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4076143