Catalytic 2,3,4-hexatriene formation by terminal alkyne coupling at calcium.
Barrett, Anthony G M; Crimmin, Mark R; Hill, Michael S; Hitchcock, Peter B; Lomas, Sarah L; Procopiou, Panayiotis A; Suntharalingam, Kogularamanan; Chemical communications (Cambridge, England) 34 (2009) 2299–2301; doi:10.1039/b818848c

data_7104348
_publ_section_title
;
 Catalytic 2,3,4-hexatriene formation by terminal alkyne coupling at
 calcium.
;
_journal_issue                   17
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2299
_journal_page_last               2301
_journal_paper_doi               10.1039/b818848c
_journal_volume                  34
_journal_year                    2009
_chemical_formula_moiety         'C66 H92 Ca2 N4 O2, C7 H8'
_chemical_formula_sum            'C73 H100 Ca2 N4 O2'
_chemical_formula_weight         1145.73
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                91.5190(10)
_cell_angle_beta                 104.5370(10)
_cell_angle_gamma                115.6400(10)
_cell_formula_units_Z            2
_cell_length_a                   13.2296(2)
_cell_length_b                   14.3726(3)
_cell_length_c                   21.2865(4)
_cell_measurement_reflns_used    28675
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.022
_cell_measurement_theta_min      3.395
_cell_volume                     3489.52(11)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo & Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_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  0.0546
_diffrn_reflns_av_sigmaI/netI    0.0489
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            54730
_diffrn_reflns_theta_full        26.06
_diffrn_reflns_theta_max         26.06
_diffrn_reflns_theta_min         3.53
_exptl_absorpt_coefficient_mu    0.208
_exptl_absorpt_correction_T_max  0.9531
_exptl_absorpt_correction_T_min  0.9018
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.090
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1244
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.661
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     751
_refine_ls_number_reflns         13704
_refine_ls_number_restraints     91
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0497
_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^)+(0.0554P)^2^+1.8004P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1154
_refine_ls_wR_factor_ref         0.1295
_reflns_number_gt                10031
_reflns_number_total             13704
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b818848c.txt
_cod_data_source_block           jul1207
_cod_database_code               7104348