Reaction of Cp*2Zr(2,3-dimethylbutadiene) with Isonitriles and CO
Valadez, Travis N.; Norton, Jack R.; Neary, Michelle C.; Quinlivan, Patrick J.; Organometallics 35 (2016) 3163–; doi:10.1021/acs.organomet.6b00522

data_4086729
_publ_section_title
;
 Reaction of Cp*2Zr(2,3-dimethylbutadiene) with Isonitriles and CO
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              3163
_journal_paper_doi               10.1021/acs.organomet.6b00522
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C31 H49 N Zr'
_chemical_formula_sum            'C31 H49 N Zr'
_chemical_formula_weight         526.93
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.033(2)
_cell_length_b                   14.892(2)
_cell_length_c                   25.247(4)
_cell_measurement_reflns_used    9161
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      32.99
_cell_measurement_theta_min      2.51
_cell_volume                     5652.1(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0597
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            98275
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         32.997
_diffrn_reflns_theta_min         1.613
_exptl_absorpt_coefficient_mu    0.407
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6824
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_description       plate
_exptl_crystal_F_000             2256
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.805
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         10415
_refine_ls_number_restraints     570
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0353
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0311P)^2^+5.3766P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0776
_refine_ls_wR_factor_ref         0.0872
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7917
_reflns_number_total             10415
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00522_si_002.cif
_cod_data_source_block           zrcntbu
_cod_original_cell_volume        5652.1(15)
_cod_database_code               4086729
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.902
_shelx_estimated_absorpt_t_max   0.980
_shelx_res_checksum              80936
_shelx_hkl_checksum              55755