Variable Coordination Modes of Hydrotris(3-isopropyl-4-bromopyrazolyl)borate (Tp') in Fe(II), Mn(II), Cr(II), and Cr(III) Complexes: Formation of MTp'Cl (M = Fe and Mn), Structural Isomerism in CrTp'2, and the Observation of Tp'- as an Uncoordinated Anion
Tim J. Brunker; Tony Hascall; Andrew R. Cowley; Leigh H. Rees; Dermot O'Hare; Inorganic Chemistry 40 (2001) 3170–3176; doi:10.1021/ic010125k

data_4319879
_publ_contact_author
;
Prof. Dermot O'Hare
Inorganic Chemistry Laboratory
University of Oxford
South Parks Rd.
Oxford
OX1 3QR
;
_publ_contact_author_email       'dermot.ohare@chem.ox.ac.uk '
_publ_contact_author_fax         ' +44 1865 272 690 '
_publ_contact_author_phone       ' +44 1865 272 658 '
_publ_section_title
;
 Variable Coordination Modes of
 Hydrotris(3-isopropyl-4-bromopyrazolyl)borate (Tp') in Fe(II), Mn(II),
 Cr(II), and Cr(III) Complexes: Formation of MTp'Cl (M = Fe and Mn),
 Structural Isomerism in CrTp'2, and the Observation of Tp'- as an
 Uncoordinated Anion
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3170
_journal_page_last               3176
_journal_paper_doi               10.1021/ic010125k
_journal_volume                  40
_journal_year                    2001
_chemical_compound_source
;
         ?
;
_chemical_formula_moiety         ' C72 H93 B3 Br9 Cr1 N18'
_chemical_formula_sum            'C72 H93 B3 Br9 Cr N18'
_chemical_formula_weight         2014.23
_chemical_melting_point          ?
_chemical_name_systematic
;
         ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_conform_dict_location     ftp://ftp.iucr.org/cifdics/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1
_audit_creation_date             2001-01-24T16:53:36-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                86.300(3)
_cell_angle_beta                 81.231(3)
_cell_angle_gamma                62.911(2)
_cell_formula_units_Z            2
_cell_length_a                   12.5760(10)
_cell_length_b                   12.7600(10)
_cell_length_c                   29.9640(10)
_cell_measurement_reflns_used    20247
_cell_measurement_temperature    150
_cell_measurement_theta_max      23.5
_cell_measurement_theta_min      0
_cell_volume                     4230.7(5)
_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
;
  CAMERON (Watkin, Prout & Pearce,  1996)
;
_computing_publication_material
;
         CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)
;
_computing_structure_refinement
;
         CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)
;
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'
_diffrn_ambient_temperature      150
_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  0.041
_diffrn_reflns_number            20247
_diffrn_reflns_theta_max         23.5
_diffrn_reflns_theta_min         0
_exptl_absorpt_coefficient_mu    4.44
_exptl_absorpt_correction_T_max  0.17
_exptl_absorpt_correction_T_min  0.17
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            ' pale orange'
_exptl_crystal_density_diffrn    1.58
_exptl_crystal_density_meas      ?
_exptl_crystal_description       ' block'
_exptl_crystal_F_000             2004.33
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.97
_refine_diff_density_min         -0.89
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.11
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     953
_refine_ls_number_reflns         8452
_refine_ls_R_factor_gt           0.054
_refine_ls_shift/su_max          0.701E-3
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Chebychev polynomial with 4 parameters, Carruthers & Watkin , 1979,
  6.96     4.01     6.38     2.37
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0426
_reflns_number_gt                8452
_reflns_number_total             11270
_reflns_threshold_expression     >3.00\s(I)
_cod_data_source_file            ic010125k_1.cif
_cod_data_source_block           arc8b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 
;
_cod_original_cell_volume        4230.7
_cod_original_formula_sum        ' C72 H93 B3 Br9 Cr1 N18'
_cod_database_code               4319879