Cycloaddition of Coordinated Diazoalkanes to Ethene To Yield 3H-Pyrazole Derivatives
Albertin, Gabriele; Antoniutti, Stefano; Baldan, Daniela; Castro, Jesús; Comparin, Giulia; Organometallics 32 (2013) 3157–; doi:10.1021/om4004016

data_4089541
_publ_section_title
;
 Cycloaddition of Coordinated Diazoalkanes to Ethene To Yield 3H-Pyrazole
 Derivatives
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              3157
_journal_paper_doi               10.1021/om4004016
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C66 H63 B Cl2 N2 O3 P2 Ru'
_chemical_formula_weight         1176.90
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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                102.032(2)
_cell_angle_beta                 109.350(2)
_cell_angle_gamma                96.688(2)
_cell_formula_units_Z            2
_cell_length_a                   12.3858(16)
_cell_length_b                   14.1762(19)
_cell_length_c                   18.603(3)
_cell_measurement_reflns_used    5203
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.41
_cell_measurement_theta_min      2.16
_cell_volume                     2952.6(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP 3 for Windows (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       '\f and \w 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  0.0399
_diffrn_reflns_av_sigmaI/netI    0.0778
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            28046
_diffrn_reflns_theta_full        28.07
_diffrn_reflns_theta_max         28.07
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    0.458
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6890
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1220
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.943
_refine_diff_density_min         -0.629
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     686
_refine_ls_number_reflns         13968
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.1088
_refine_ls_R_factor_gt           0.0519
_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^)+(0.0648P)^2^+1.3588P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1193
_refine_ls_wR_factor_ref         0.1482
_reflns_number_gt                8359
_reflns_number_total             13968
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om4004016_si_002.cif
_cod_data_source_block           3b
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        2952.5(7)
_cod_original_sg_symbol_H-M      'P-1   '
_cod_original_formula_sum        'C66 H63 B1 Cl2 N2 O3 P2 Ru'
_cod_database_code               4089541