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

data_7003863
_publ_section_title
;
 En route to zirconium hydrazides(2&#x2212;)
;
_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            'C23 H48 Cl N5 Si2 Zr'
_chemical_formula_weight         577.51
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                ga_hh7
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.439(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.583(3)
_cell_length_b                   15.613(4)
_cell_length_c                   20.578(6)
_cell_measurement_temperature    100(2)
_cell_volume                     3073.3(15)
_computing_cell_refinement       'SAINT (Bruker AXS, 1997-2006)'
_computing_data_collection       'SMART (Bruker AXS, 1997-2003)'
_computing_data_reduction        'SAINT (Bruker AXS, 1997-2006)'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'CCD area detector (Bruker AXS Smart 1000)'
_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  0.0606
_diffrn_reflns_av_sigmaI/netI    0.0415
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            77762
_diffrn_reflns_theta_full        32.10
_diffrn_reflns_theta_max         32.10
_diffrn_reflns_theta_min         1.64
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.541
_exptl_absorpt_correction_T_max  0.8923
_exptl_absorpt_correction_T_min  0.8760
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2004-2007)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.622
_refine_diff_density_min         -0.548
_refine_diff_density_rms         0.091
_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   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     306
_refine_ls_number_reflns         10414
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0379
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0446P)^2^+1.1419P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.0956
_reflns_number_gt                7730
_reflns_number_total             10414
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b800682b.txt
_cod_data_source_block           complex_2a
_cod_original_cell_volume        3073.5(14)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7003863
_audit_block_refno               316