Crystal structure of bis{μ~2~-[(2-iminocyclopentylidene)methylidene]azanido-κ^2^<i>N</i>:<i>N</i>'}bis[(η^5^-pentamethylcyclopentadienyl)zirconium(IV)] hexane monosolvate
Becker, Lisanne; Spannenberg, Anke; Arndt, Perdita; Rosenthal, Uwe; Acta Crystallographica Section E 71 (2015) m219–m220; doi:10.1107/S2056989015021234

data_2241322
_publ_section_title
;
 Crystal structure of
 bis{\m~2~-[(2-iminocyclopentylidene)methylidene]azanido-\k^2^<i>N</i>:<i>N</i>'}bis[(\h^5^-pentamethylcyclopentadienyl)zirconium(IV)]
 hexane monosolvate
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m219
_journal_page_last               m220
_journal_paper_doi               10.1107/S2056989015021234
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Zr2 (C10 H15)4 (C6 H6 N2)2], C6 H14'
_chemical_formula_moiety         'C52 H72 N4 Zr2, C6 H14'
_chemical_formula_sum            'C58 H86 N4 Zr2'
_chemical_formula_weight         1021.74
_chemical_name_systematic
;Bis{\m~2~-[(2-iminocyclopentylidene)methylidene]azanido-\k^2^<i>N</i>:<i>N</i>'}bis[(\h^5^-pentamethylcyclopentadienyl)zirconium(IV)]
hexane monosolvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 117.7232(15)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.4862(8)
_cell_length_b                   16.9048(11)
_cell_length_c                   13.0151(8)
_cell_measurement_reflns_used    9621
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.80
_cell_measurement_theta_min      2.95
_cell_volume                     2626.6(3)
_computing_cell_refinement
;
SAINT (Bruker, 2014)
;
_computing_data_collection
;
APEX2 (Bruker, 2014)
;
_computing_data_reduction
;
SAINT (Bruker, 2014)
;
_computing_molecular_graphics
;
XP in SHELXTL (Sheldrick, 2008) and Mercury (Macrae <i>et al.</i>,
2006)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            60472
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_min         1.706
_exptl_absorpt_coefficient_mu    0.437
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.88
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Bruker, 2014)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_description       prism
_exptl_crystal_F_000             1084
_exptl_crystal_size_max          0.345
_exptl_crystal_size_mid          0.268
_exptl_crystal_size_min          0.177
_refine_diff_density_max         0.883
_refine_diff_density_min         -0.426
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         6341
_refine_ls_number_restraints     239
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0352
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0437P)^2^+3.0941P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0883
_refine_ls_wR_factor_ref         0.0944
_reflns_number_gt                5621
_reflns_number_total             6341
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5234sup1.cif
_cod_data_source_block           I
_cod_database_code               2241322
_shelx_hkl_checksum              20897
_shelx_res_checksum              49756
_cod_database_fobs_code 2241322