Cycloaddition reactions of transition metal hydrazides with alkynes and heteroalkynes: coupling of Ti=NNPh2 with PhCCMe, PhCCH, MeCN and tBuCP.
Selby, Jonathan D; Schulten, Christian; Schwarz, Andrew D; Stasch, Andreas; Clot, Eric; Jones, Cameron; Mountford, Philip; Chemical communications (Cambridge, England)  (2008) 5101–5103; doi:10.1039/b813911c

data_7103464
_publ_section_title
;
 Cycloaddition reactions of transition metal hydrazides with alkynes
 and heteroalkynes: coupling of Ti=NNPh2 with PhCCMe, PhCCH, MeCN and
 tBuCP.
;
_journal_issue                   41
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              5101
_journal_page_last               5103
_journal_paper_doi               10.1039/b813911c
_journal_year                    2008
_chemical_formula_moiety         'C58 H84 N12 Si4 Ti2, 0.8 C6H6'
_chemical_formula_sum            'C62.8 H88.8 N12 Si4 Ti2'
_chemical_formula_weight         1220.02
_chemical_name_systematic
;
Ti2(N2Npy)2{u-N(NPh2)C(Me)N}2 . 0.8 C6H6
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           CRYSTALS_ver_12.84
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            9
_cell_length_a                   40.0450(3)
_cell_length_b                   40.0450(3)
_cell_length_c                   11.26710(10)
_cell_measurement_reflns_used    7932
_cell_measurement_temperature    150
_cell_measurement_theta_max      28
_cell_measurement_theta_min      5
_cell_volume                     15647.3(2)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'USER DEFINED STRUCTURE SOLUTION'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.023
_diffrn_reflns_limit_h_max       52
_diffrn_reflns_limit_h_min       -52
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15799
_diffrn_reflns_theta_full        26.974
_diffrn_reflns_theta_max         27.524
_diffrn_reflns_theta_min         5.141
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.344
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.165
_exptl_crystal_description       plate
_exptl_crystal_F_000             5846.398
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.57
_refine_diff_density_min         -0.32
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0697
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         5552
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.003
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
0.953 0.589 0.672
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0586
_refine_ls_wR_factor_gt          0.0453
_refine_ls_wR_factor_ref         0.0453
_reflns_limit_h_max              25
_reflns_limit_h_min              -51
_reflns_limit_k_max              52
_reflns_limit_k_min              0
_reflns_limit_l_max              14
_reflns_limit_l_min              0
_reflns_number_gt                5552
_reflns_number_total             7952
_reflns_threshold_expression     I>3.0\s(I)
_cod_data_source_file            b813911c.txt
_cod_data_source_block           Compound_5
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' 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      'R -3 '
_cod_original_formula_sum        'C62.80 H88.8 N12 Si4 Ti2'
_cod_database_code               7103464