Catalytic hydroacetylenation of carbodiimides with homoleptic alkaline earth hexamethyldisilazides.
Arrowsmith, Merle; Crimmin, Mark R.; Hill, Michael S.; Lomas, Sarah L.; Heng, Myra Sae; Hitchcock, Peter B.; Kociok-Köhn, Gabriele; Dalton transactions (Cambridge, England : 2003) 43 (2014) 14249–14256; doi:10.1039/c3dt53542h

data_7032514
_publ_section_title
;
 Catalytic hydroacetylenation of carbodiimides with homoleptic alkaline
 earth hexamethyldisilazides.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14249
_journal_page_last               14256
_journal_paper_doi               10.1039/c3dt53542h
_journal_volume                  43
_journal_year                    2014
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C60 H76 Ca2 N8'
_chemical_formula_sum            'C60 H76 Ca2 N8'
_chemical_formula_weight         989.45
_chemical_name_systematic
;
 ?
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2007-03-08T10:45:08-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                96.295(2)
_cell_angle_beta                 94.289(1)
_cell_angle_gamma                93.976(1)
_cell_formula_units_Z            2
_cell_length_a                   10.8208(3)
_cell_length_b                   16.1524(4)
_cell_length_c                   17.4648(3)
_cell_measurement_reflns_used    25901
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.022
_cell_measurement_theta_min      3.395
_cell_measurement_wavelength     0.71073
_cell_volume                     3016.36(12)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and 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_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.681538E-1
_diffrn_orient_matrix_UB_12      -0.48347E-2
_diffrn_orient_matrix_UB_13      0.408299E-1
_diffrn_orient_matrix_UB_21      -0.62138E-1
_diffrn_orient_matrix_UB_22      -0.9546E-3
_diffrn_orient_matrix_UB_23      0.395571E-1
_diffrn_orient_matrix_UB_31      -0.11632E-1
_diffrn_orient_matrix_UB_32      -0.622826E-1
_diffrn_orient_matrix_UB_33      -0.104693E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_unetI/netI     0.0414
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            42730
_diffrn_reflns_theta_full        26.05
_diffrn_reflns_theta_max         26.05
_diffrn_reflns_theta_min         3.53
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.23
_exptl_absorpt_correction_T_max  0.9558
_exptl_absorpt_correction_T_min  0.9058
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.089
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.569
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     647
_refine_ls_number_reflns         11828
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.1012
_refine_ls_R_factor_gt           0.0716
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0991P)^2^+3.0393P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1857
_refine_ls_wR_factor_ref         0.2077
_reflns_number_gt                8508
_reflns_number_total             11828
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt53542h.txt
_cod_data_source_block           mar607
_cod_depositor_comments
'Adding full bibliography for 7032514--7032517.cif.'
_cod_database_code               7032514