Synthesis, structure, and alkyne insertion of a mixed-sandwich zirconacarborane alkyl
Liu, Dongmei; Qiu, Zaozao; Xie, Zuowei; Inorganic Chemistry Frontiers 2 (2015) 467–; doi:10.1039/C4QI00244J

data_4348431
_publ_section_title
;
 Synthesis, structure, and alkyne insertion of a mixed-sandwich
 zirconacarborane alkyl
;
_journal_issue                   5
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              467
_journal_paper_doi               10.1039/C4QI00244J
_journal_volume                  2
_journal_year                    2015
_chemical_formula_sum            'C38 H56 B9 N Si2 Zr'
_chemical_formula_weight         771.53
_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
_audit_update_record
;
2014-12-26 deposited with the CCDC.
2015-03-12 downloaded from the CCDC.
;
_cell_angle_alpha                91.666(3)
_cell_angle_beta                 91.912(3)
_cell_angle_gamma                114.031(3)
_cell_formula_units_Z            2
_cell_length_a                   10.1753(19)
_cell_length_b                   11.110(2)
_cell_length_c                   22.337(4)
_cell_measurement_reflns_used    4660
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.19
_cell_measurement_theta_min      2.29
_cell_volume                     2302.5(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0244
_diffrn_reflns_av_sigmaI/netI    0.0561
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            11595
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    0.316
_exptl_absorpt_correction_T_max  0.8863
_exptl_absorpt_correction_T_min  0.7685
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            prism
_exptl_crystal_density_diffrn    1.113
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       yellow
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.359
_refine_diff_density_min         -1.497
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.956
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         7965
_refine_ls_number_restraints     200
_refine_ls_restrained_S_all      0.966
_refine_ls_R_factor_all          0.0990
_refine_ls_R_factor_gt           0.0748
_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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2200
_refine_ls_wR_factor_ref         0.2421
_reflns_number_gt                6115
_reflns_number_total             7965
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4qi00244j2.cif
_cod_data_source_block           2c
_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/RSC/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_sg_symbol_H-M      P-1
_cod_database_code               4348431