Zirconocene-Mediated Macrocyclizations of Diynes Containing Di-o-Methylphenylene Spacers
Adam D. Miller; Jennifer L. McBee; T. Don Tilley; Journal of Organic Chemistry 74 (2009) 2880–2883; doi:10.1021/jo802715m

data_4024431
_publ_section_title
;
Zirconocene-Mediated Macrocyclizations of Diynes Containing
Di-o-Methylphenylene Spacers
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              2880
_journal_page_last               2883
_journal_paper_doi               10.1021/jo802715m
_journal_volume                  74
_journal_year                    2009
_chemical_formula_moiety         'C88 H96 Zr2'
_chemical_formula_sum            'C88 H96 Zr2'
_chemical_formula_weight         1336.09
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 94.963(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.5012(10)
_cell_length_b                   17.8328(17)
_cell_length_c                   17.7760(17)
_cell_measurement_reflns_used    5502
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.60
_cell_measurement_theta_min      2.46
_cell_volume                     3316.4(5)
_computing_cell_refinement       'Saint v7.06, Bruker 2004'
_computing_data_collection       'Apex2-v1.0.27, Bruker 2004'
_computing_data_reduction        'Saint v7.06, Bruker 2004'
_computing_molecular_graphics    'SHELXL-XP (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Pt 200'
_diffrn_measurement_method       \w/2\q-scans
_diffrn_radiation_monochromator  'Si-<111> channel cut crystal'
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7750
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_av_sigmaI/netI    0.0340
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            31351
_diffrn_reflns_theta_full        24.53
_diffrn_reflns_theta_max         24.53
_diffrn_reflns_theta_min         1.62
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.448
_exptl_absorpt_correction_T_max  0.288
_exptl_absorpt_correction_T_min  0.208
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs, 2004'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.085
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         5517
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0842
_refine_ls_R_factor_gt           0.0600
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0963P)^2^+4.3818P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1641
_refine_ls_wR_factor_ref         0.1848
_reflns_number_gt                3959
_reflns_number_total             5517
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo802715m_si_001.cif
_cod_data_source_block           adam10
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4024431