Reactions of a methylzirconocene cation with phosphinoalkynes: an alternative pathway for generating Cp2Zr(II) systems
Xin Xu; Roland Frohlich; Constantin G. Daniliuc; Gerald Kehr; Gerhard Erker; Chem.Commun. 48 (2012) 6109–; doi:10.1039/c2cc31883k

data_7107847
_publ_section_title
;
 Reactions of a methylzirconocene cation with phosphinoalkynes: an
 alternative pathway for generating Cp2Zr(II) systems
;
_journal_name_full               Chem.Commun.
_journal_page_first              6109
_journal_paper_doi               10.1039/c2cc31883k
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C70 H58 B F20 P Zr'
_chemical_formula_weight         1412.16
_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                81.7800(10)
_cell_angle_beta                 82.6150(10)
_cell_angle_gamma                83.2860(10)
_cell_formula_units_Z            2
_cell_length_a                   10.6745(2)
_cell_length_b                   15.6839(3)
_cell_length_c                   19.2457(3)
_cell_measurement_reflns_used    8832
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      4.08
_cell_volume                     3146.54(10)
_computing_cell_refinement       'Collect (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'XP (BrukerAXS, 2000)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Nonius KappaCCD APEXII'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Montel mirror'
_diffrn_radiation_source         'rotating anode Nonius FR591'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.045
_diffrn_reflns_av_sigmaI/netI    0.0385
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            32876
_diffrn_reflns_theta_full        28.25
_diffrn_reflns_theta_max         28.25
_diffrn_reflns_theta_min         4.09
_exptl_absorpt_coefficient_mu    0.302
_exptl_absorpt_correction_T_max  0.9791
_exptl_absorpt_correction_T_min  0.8810
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)'
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1436
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.817
_refine_diff_density_min         -0.658
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     849
_refine_ls_number_reflns         15020
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0556
_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^)+(0.0523P)^2^+3.7699P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1347
_refine_ls_wR_factor_ref         0.1443
_reflns_number_gt                13079
_reflns_number_total             15020
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc31883k.txt
_cod_data_source_block           erk6302
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7107847