Synthesis of Oligoenes that Contain up to 15 Double Bonds from 1,6-Heptadiynes
Constantin Czekelius; Jillian Hafer; Zachary J. Tonzetich; Richard R. Schrock; Ronald L. Christensen; Peter Müller; Journal of the American Chemical Society 128 (2006) 16664–16675; doi:10.1021/ja0656705

data_4111255
_publ_section_title
;
 Synthesis of Oligoenes that Contain up to 15 Double Bonds from
 1,6-Heptadiynes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16664
_journal_page_last               16675
_journal_paper_doi               10.1021/ja0656705
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C55.5 H68 F24 Mo2 N2 O8'
_chemical_formula_weight         1539.00
_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                 90.8330(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.0704(4)
_cell_length_b                   27.1993(10)
_cell_length_c                   22.5569(9)
_cell_measurement_reflns_used    7082
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.01
_cell_measurement_theta_min      2.42
_cell_volume                     6791.3(4)
_computing_cell_refinement       'SAINT 5 (Bruker-AXS, 2003)'
_computing_data_collection       'SMART 5 (Bruker-AXS, 2003)'
_computing_data_reduction        'SAINT 5 (Bruker-AXS, 2003)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       'omega and phi scans'
_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  0.0699
_diffrn_reflns_av_sigmaI/netI    0.0453
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            135769
_diffrn_reflns_theta_full        28.70
_diffrn_reflns_theta_max         28.70
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    0.484
_exptl_absorpt_correction_T_max  0.9623
_exptl_absorpt_correction_T_min  0.9180
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_description       block
_exptl_crystal_F_000             3116
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.613
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     913
_refine_ls_number_reflns         17523
_refine_ls_number_restraints     131
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0767
_refine_ls_R_factor_gt           0.0485
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0620P)^2^+7.6779P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1199
_refine_ls_wR_factor_ref         0.1332
_reflns_number_gt                12876
_reflns_number_total             17523
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0656705si20060814_111031_2.cif
_cod_data_source_block           05196
_cod_original_formula_sum        'C55.50 H68 F24 Mo2 N2 O8'
_cod_database_code               4111255