New Diamide-Diamine Ligands and their Zirconium and Hafnium Dichloride and Bis(dimethylamide) Complexes
Michael E. G. Skinner; Yahong Li; Philip Mountford; Inorganic Chemistry 41 (2002) 1110–1119; doi:10.1021/ic011043z

data_4317659
_publ_contact_author
;
  Dr P. Mountford
  Inorganic Chemistry Laboratory
  South Parks Road
  Oxford
  OX1 3QR
  UK
;
_publ_contact_author_email       Philip.Mountford@chem.ox.ac.uk
_publ_contact_author_fax         '+44 1865 272690'
_publ_contact_author_phone       '+44 1865 272679'
_publ_section_title
;
 New Diamide-Diamine Ligands and their Zirconium and Hafnium Dichloride
 and Bis(dimethylamide) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1110
_journal_page_last               1119
_journal_paper_doi               10.1021/ic011043z
_journal_volume                  41
_journal_year                    2002
_chemical_compound_source
;
  H2N2NN' recrystallised  from EtOH
;
_chemical_formula_moiety         ' C24 H30 N4 S2 O4 , C2H6O '
_chemical_formula_sum            'C26 H36 N4 O5 S2'
_chemical_formula_weight         548.72
_chemical_name_systematic
;
  (2-C5H4N)CH2N{CH2CH2N(H)Ts}2.EtOH
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   'Fourier maps and geometric'
_atom_sites_solution_primary     'direct methods (SIR92)'
_cell_angle_alpha                90
_cell_angle_beta                 105.271(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.9180(5)
_cell_length_b                   13.6490(5)
_cell_length_c                   25.9760(6)
_cell_measurement_reflns_used    37411
_cell_measurement_temperature    175
_cell_measurement_theta_max      27
_cell_measurement_theta_min      0
_cell_volume                     5786.4(3)
_computing_cell_refinement
;
DIP2000 software 'DENZO' (Otwinowski & Minor, 1996)
;
_computing_data_collection       'DIP2000 software "Xpress" (MAC Science, 1989)'
_computing_data_reduction
;
DIP2000 software 'DENZO' (Otwinowski & Minor, 1996)
;
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 1994)'
_computing_publication_material
;
CRYSTALS Issue 10 (Watkin et al, 1996)
;
_computing_structure_refinement
;
CRYSTALS Issue 10 (Watkin et al, 1996)
;
_computing_structure_solution    'SIR92 (Altomare, et al, 1994)'
_diffrn_ambient_temperature      175
_diffrn_measurement_device_type  'Enraf-nonius DIP2000'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_sigmaI/netI    0.0992
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            37411
_diffrn_reflns_theta_max         26.49
_diffrn_reflns_theta_min         1.30
_diffrn_standards_decay_%        'not measured'
_diffrn_standards_interval_count 'not measured'
_diffrn_standards_interval_time  'not measured'
_diffrn_standards_number         'not measured'
_exptl_absorpt_coefficient_mu    0.21
_exptl_absorpt_correction_T_max  0.900
_exptl_absorpt_correction_T_min  0.891
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.26
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             2336
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.55
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.71
_refine_diff_density_min         -0.41
_refine_ls_abs_structure_Flack   none
_refine_ls_extinction_coef       240.6(570)
_refine_ls_extinction_method     'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_obs   1.0339
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           blocked
_refine_ls_number_parameters     693
_refine_ls_number_reflns         7331
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0386
_refine_ls_shift/esd_max         0.010
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      'Chebychev polynomial'
_refine_ls_wR_factor_obs         0.0469
_reflns_limit_h_max              20
_reflns_limit_h_min              -21
_reflns_limit_k_max              17
_reflns_limit_k_min              0
_reflns_limit_l_max              32
_reflns_limit_l_min              0
_reflns_number_observed          7331
_reflns_number_total             21683
_reflns_observed_criterion       >3\s(I)
_cod_data_source_file            ic011043z_2.cif
_cod_data_source_block           COMPOUND_2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic ' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

data name '_diffrn_measurement_device-type' was replaced with
'_diffrn_measurement_device_type' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_cell_volume        5786.4
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        ' C26 H36 N4 S2 O5 '
_cod_database_code               4317659