[Bis(pyridin-2-ylmethyl) ether]trichloridorhodium(III) dichloromethane monosolvate: unusual hydrolysis of the methylene bridge in (pyrazolylmethyl)pyridine
Ojwach, Stephen O.; Omondi, Bernard; Darkwa, James; Acta Crystallographica Section E 67 (2011) m1097–; doi:10.1107/S1600536811027644

data_2231242
_publ_section_title
;
 [Bis(pyridin-2-ylmethyl) ether]trichloridorhodium(III) dichloromethane
 monosolvate: unusual hydrolysis of the methylene bridge in
 (pyrazolylmethyl)pyridine
;
_journal_coeditor_code           OM2440
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1097
_journal_paper_doi               10.1107/S1600536811027644
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Rh Cl3 (C12 H12 N2 O)], C H2 Cl2'
_chemical_formula_moiety         'C12 H12 Cl3 N2 O Rh, C H2 Cl2'
_chemical_formula_sum            'C13 H14 Cl5 N2 O Rh'
_chemical_formula_weight         494.42
_chemical_name_systematic
;
[Bis(pyridin-2-ylmethyl) ether]trichloridorhodium(III) dichloromethane
monosolvate
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 95.071(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5360(18)
_cell_length_b                   12.527(2)
_cell_length_c                   14.340(3)
_cell_measurement_reflns_used    31705
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.57
_cell_measurement_theta_min      2.14
_cell_volume                     1706.3(6)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT-Plus and XPREP (Bruker, 2007)'
_computing_molecular_graphics
'DIAMOND (Brandenburg & Putz, 2005) and ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker X8 APEXII 4K KappaCCD'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1021
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            30694
_diffrn_reflns_theta_full        28.57
_diffrn_reflns_theta_max         28.57
_diffrn_reflns_theta_min         2.14
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.784
_exptl_absorpt_correction_T_max  0.9161
_exptl_absorpt_correction_T_min  0.7883
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.925
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.498
_refine_diff_density_min         -1.247
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         4276
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.09
_refine_ls_R_factor_gt           0.0479
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0602P)^2^+6.0697P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.114
_refine_ls_wR_factor_ref         0.1392
_reflns_number_gt                2925
_reflns_number_total             4276
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om2440.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2231242
_cod_database_fobs_code          2231242