An organometallic Rh^III^ complex with a distorted octahedral structure: (acetonitrile-κ<i>N</i>)dimethyl(1,4,7-trimethyl-1,4,7-triazacyclononane-κ^3^<i>N</i>,<i>N</i>',<i>N</i>'')rhodium(III) tetraphenylborate
Fooladi, Erik; Dalhus, Bjørn; Rømming, Christian; Tilset, Mats; Acta Crystallographica Section C 58 (2002) m567–m569; doi:10.1107/S0108270102019182

data_2013084
_publ_section_title
;An organometallic Rh^III^ complex with a distorted octahedral structure:
 (acetonitrile-\k<i>N</i>)dimethyl(1,4,7-trimethyl-1,4,7-triazacyclononane-\k^3^<i>N</i>,<i>N</i>',<i>N</i>'')rhodium(III)
 tetraphenylborate
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m567
_journal_page_last               m569
_journal_paper_doi               10.1107/S0108270102019182
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac
'[Rh (C H3)2 (C2 H3 N) (C9 H21 N3)] [B(C6 H5)4]'
_chemical_formula_moiety         'C13 H30 N4 Rh + , C24 H20 B -'
_chemical_formula_structural     'C13 H30 N4 Rh + , C24 H20 B -'
_chemical_formula_sum            'C37 H50 B N4 Rh'
_chemical_formula_weight         664.53
_chemical_name_systematic
;
(acetonitrile-\kN)dimethyl(1,4,7-trimethyl-1,4,7-triazacyclononane-
\k^3^N)rhodium(III) tetraphenylborate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90
_cell_angle_beta                 92.7890(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2560(3)
_cell_length_b                   16.6074(3)
_cell_length_c                   14.6189(3)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      40.37
_cell_measurement_theta_min      2.30
_cell_volume                     3457.00(12)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 1995)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.937
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device_type  'Siemens SMART CCD area-detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.017
_diffrn_reflns_av_sigmaI/netI    0.022
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            55207
_diffrn_reflns_theta_full        40.37
_diffrn_reflns_theta_max         40.37
_diffrn_reflns_theta_min         2.30
_exptl_absorpt_coefficient_mu    0.524
_exptl_absorpt_correction_T_max  0.85
_exptl_absorpt_correction_T_min  0.73
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.74
_refine_diff_density_min         -0.64
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.210
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         20545
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.210
_refine_ls_R_factor_all          0.044
_refine_ls_R_factor_gt           0.032
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.02P)^2^+1.41P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.069
_refine_ls_wR_factor_ref         0.077
_reflns_number_gt                17370
_reflns_number_total             20545
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ob1087.cif
_cod_data_source_block           I
_cod_depositor_comments
;
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        3457.00(10)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2013084
_cod_database_fobs_code          2013084