Crystal structures of di-μ-bromido-bis{dibromido[η^5^-2-(dimethylamino)indenyl]zirconium(IV)} and dibromidobis[η^5^-2-(dimethylamino)indenyl]zirconium(IV)
Medvedev, Michael G.; Borisov, Ilya S.; Kulyabin, Pavel S.; Izmer, Vyatcheslav V.; Kononovich, Dmitry S.; Uborsky, Dmitry V.; Voskoboynikov, Alexander Z.; Acta Crystallographica Section E 72 (2016) 1599–1602; doi:10.1107/S2056989016016595

data_2241892
_publ_section_title
;
 Crystal structures of
 di-\m-bromido-bis{dibromido[\h^5^-2-(dimethylamino)indenyl]zirconium(IV)}
 and dibromidobis[\h^5^-2-(dimethylamino)indenyl]zirconium(IV)
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1599
_journal_page_last               1602
_journal_paper_doi               10.1107/S2056989016016595
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          '[Zr2 Br6 (C11 H12 N)2]'
_chemical_formula_moiety         'C22 H24 Br6 N2 Zr2'
_chemical_formula_sum            'C22 H24 Br6 N2 Zr2'
_chemical_formula_weight         978.33
_chemical_name_common
di[(\m-bromo)(\h^5^-2-dimethylaminoindenyl)dibromozirconium(IV)]
_chemical_name_systematic
;
Di-\m-bromido-bis{dibromido[\h^5^-2-(dimethylamino)indenyl]zirconium(IV)}
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.16 svn.r3265 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 99.0280(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3275(6)
_cell_length_b                   13.9365(7)
_cell_length_c                   17.6082(9)
_cell_measurement_reflns_used    9986
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      35.28
_cell_measurement_theta_min      2.33
_cell_volume                     2745.3(2)
_computing_cell_refinement
;
SAINT (Bruker, 2009)
;
_computing_data_collection
;
APEX2 (Bruker, 2012)
;
_computing_data_reduction
;
SAINT (Bruker, 2009)
;
_computing_molecular_graphics
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            35046
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.998
_diffrn_reflns_theta_min         1.873
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.507
_exptl_absorpt_correction_T_max  0.1654
_exptl_absorpt_correction_T_min  0.0520
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Bruker, 2008)
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_density_diffrn    2.367
_exptl_crystal_description       plate
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.226
_refine_diff_density_min         -0.801
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         7921
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0327
_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^)+(0.0301P)^2^+4.7762P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0696
_refine_ls_wR_factor_ref         0.0750
_reflns_number_gt                6465
_reflns_number_total             7921
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5329sup1.cif
_cod_data_source_block           I
_cod_database_code               2241892
_shelx_estimated_absorpt_t_min   0.140
_shelx_estimated_absorpt_t_max   0.702
_shelx_hkl_checksum              85491
_shelx_res_checksum              66829