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_4319883
_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_formula_moiety         'C18 H25 B1 Br3 Cl1 Cr1 N6'
_chemical_formula_sum            'C38.5 H56 B2 Br6 Cr N12'
_chemical_formula_weight         1240.03
_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             2001-01-24T15:18:48-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                98.032(4)
_cell_angle_beta                 105.392(3)
_cell_angle_gamma                101.759(3)
_cell_formula_units_Z            2
_cell_length_a                   12.9820(8)
_cell_length_b                   13.0650(9)
_cell_length_c                   15.9270(7)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     2495.5(3)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.914
_diffrn_measured_fraction_theta_max 0.914
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0
_diffrn_reflns_av_unetI/netI     0.0576
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9361
_diffrn_reflns_theta_full        26.41
_diffrn_reflns_theta_max         26.41
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    5.074
_exptl_absorpt_correction_T_max  0.4041
_exptl_absorpt_correction_T_min  0.3108
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
  ?
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.65
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1230
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.984
_refine_diff_density_min         -0.872
_refine_diff_density_rms         0.089
_refine_ls_extinction_coef       0.00000(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     562
_refine_ls_number_reflns         9361
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0729
_refine_ls_R_factor_gt           0.0417
_refine_ls_shift/su_max          0.165
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; calc
  [1.00000+0.00000exp(0.00(sin\q/\l)^2^)]/
    [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0570P)^2^+0.0400sin\q/\l]
  where P = 0.33333Fo^2^ + 0.66667Fc^2^
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1007
_refine_ls_wR_factor_ref         0.1108
_reflns_number_gt                6175
_reflns_number_total             9361
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010125k_5.cif
_cod_data_source_block           tjb1
_cod_original_formula_sum        'C38.50 H56 B2 Br6 Cr N12'
_cod_database_code               4319883
_exptl_absorpt_factor_mur        1.014
_exptl_absorpt_correction_t_ave  0.3579