En route to zirconium hydrazides(2−)
Herrmann, Heike; Wadepohl, Hubert; Gade, Lutz H.; Dalton Transactions  (2008) 2111–2119; doi:10.1039/b800682b

data_7003865
_publ_section_title
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 En route to zirconium hydrazides(2&#x2212;)
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_journal_issue                   16
_journal_name_full               'Dalton Transactions'
_journal_page_first              2111
_journal_page_last               2119
_journal_paper_doi               10.1039/b800682b
_journal_year                    2008
_chemical_formula_sum            'C28 H50 Cl N5 Si2 Zr'
_chemical_formula_weight         639.58
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_block_code                ga_hh27
_audit_creation_method           SHELXL-97
_cell_angle_alpha                70.93(3)
_cell_angle_beta                 85.85(3)
_cell_angle_gamma                74.74(3)
_cell_formula_units_Z            4
_cell_length_a                   13.360(3)
_cell_length_b                   15.968(3)
_cell_length_c                   16.930(3)
_cell_measurement_temperature    170(2)
_cell_volume                     3292.8(14)
_computing_molecular_graphics    'PLATON (Spek, 1980-2005)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF (Beurskens, 1999-2007)'
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'CCD area detector (Nonius Kappa CCD)'
_diffrn_measurement_method       '\f- and \w-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_sigmaI/netI    0.0292
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            61069
_diffrn_reflns_theta_full        27.76
_diffrn_reflns_theta_max         27.76
_diffrn_reflns_theta_min         1.40
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.513
_exptl_absorpt_correction_T_max  0.9044
_exptl_absorpt_correction_T_min  0.8212
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2004-2007)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.758
_refine_diff_density_rms         0.114
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     699
_refine_ls_number_reflns         15160
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0292
_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^)+(0.0376P)^2^+1.2874P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0752
_refine_ls_wR_factor_ref         0.0784
_reflns_number_gt                13082
_reflns_number_total             15160
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b800682b.txt
_cod_data_source_block           complex_4a
_cod_original_cell_volume        3292.8(11)
_cod_database_code               7003865
_audit_block_refno               636