#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:58:48 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179402 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/99/4329977.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4329977
loop_
_publ_author_name
'Romain J. Adcock'
'Duc Hanh Nguyen'
'Sonia Ladeira'
'Carole Le Berre'
'Philippe Serp'
'Philippe Kalck'
_publ_section_title
;
 Reactivity of Rhodium(I) Complexes Bearing Nitrogen-Containing Ligands
 toward CH3I: Synthesis and Full Characterization of Neutral
 cis-[RhX(CO)2(L)] and Acetyl [RhI(μ-I)(COMe)(CO)(L)]2 Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8670
_journal_page_last               8685
_journal_paper_doi               10.1021/ic2019988
_journal_volume                  51
_journal_year                    2012
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C5 H4 Cl N2 O2 Rh'
_chemical_formula_sum            'C5 H4 Cl N2 O2 Rh'
_chemical_formula_weight         262.46
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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
_cell_angle_alpha                90
_cell_angle_beta                 125.835(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4119(11)
_cell_length_b                   6.7619(7)
_cell_length_c                   13.9762(11)
_cell_measurement_reflns_used    7403
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      30.52
_cell_measurement_theta_min      2.41
_cell_measurement_wavelength     0.71073
_cell_volume                     797.72(14)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device_type  'Bruker Kappa APEX II'
_diffrn_measurement_method       ω-φ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0185
_diffrn_reflns_av_unetI/netI     0.0144
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10111
_diffrn_reflns_theta_full        30.52
_diffrn_reflns_theta_max         30.52
_diffrn_reflns_theta_min         2.93
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.423
_exptl_absorpt_correction_T_max  0.785
_exptl_absorpt_correction_T_min  0.670
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.185
_exptl_crystal_description       plate
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.4
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       0.0157(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     104
_refine_ls_number_reflns         2445
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0149
_refine_ls_R_factor_gt           0.0134
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0178P)²+0.1784P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0353
_refine_ls_wR_factor_ref         0.0363
_reflns_number_gt                2302
_reflns_number_total             2445
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2019988_si_002_03.cif
_cod_data_source_block           3e
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4329977
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Rh1 Rh 1.008265(10) 0.386751(12) 0.744981(7) 0.02259(4) Uani 1 1 d .
Cl1 Cl 1.13284(4) 0.39360(4) 0.95084(3) 0.02867(7) Uani 1 1 d .
O2 O 0.85522(15) 0.39898(14) 0.48615(10) 0.0434(3) Uani 1 1 d .
O1 O 1.32835(15) 0.37520(16) 0.79552(15) 0.0581(4) Uani 1 1 d .
N1 N 0.78633(12) 0.38176(12) 0.71423(9) 0.02287(19) Uani 1 1 d .
N2 N 0.76730(12) 0.41946(15) 0.79948(9) 0.0270(2) Uani 1 1 d D
H2A H 0.8517(14) 0.439(2) 0.8701(9) 0.032 Uiso 1 1 d D
C5 C 0.64081(15) 0.34298(19) 0.61789(11) 0.0322(3) Uani 1 1 d .
H5 H 0.6166 0.3108 0.5428 0.039 Uiso 1 1 calc R
C4 C 0.53012(15) 0.35619(19) 0.64277(13) 0.0367(3) Uani 1 1 d .
H4 H 0.419 0.3355 0.5899 0.044 Uiso 1 1 calc R
C3 C 0.61529(15) 0.4054(2) 0.75960(13) 0.0346(3) Uani 1 1 d .
H3 H 0.5742 0.4259 0.8042 0.042 Uiso 1 1 calc R
C2 C 0.91402(18) 0.39272(16) 0.58434(13) 0.0299(3) Uani 1 1 d .
C1 C 1.20587(19) 0.38190(17) 0.77449(16) 0.0361(3) Uani 1 1 d .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Rh1 0.02217(6) 0.02134(6) 0.02779(6) -0.00167(3) 0.01661(4) -0.00078(3)
Cl1 0.02191(13) 0.03138(14) 0.02481(13) -0.00092(9) 0.00925(11) 0.00338(9)
O2 0.0659(8) 0.0361(5) 0.0370(5) -0.0037(4) 0.0350(6) -0.0030(4)
O1 0.0423(7) 0.0518(7) 0.0996(11) -0.0167(6) 0.0524(8) -0.0080(4)
N1 0.0197(4) 0.0255(5) 0.0220(4) 0.0022(3) 0.0114(4) 0.0004(3)
N2 0.0198(4) 0.0377(5) 0.0237(4) 0.0028(4) 0.0128(4) 0.0001(4)
C5 0.0249(6) 0.0368(6) 0.0255(5) 0.0005(5) 0.0094(5) -0.0030(5)
C4 0.0188(5) 0.0423(7) 0.0378(7) 0.0077(5) 0.0103(5) -0.0011(4)
C3 0.0233(6) 0.0437(7) 0.0399(7) 0.0087(5) 0.0203(5) 0.0025(5)
C2 0.0390(7) 0.0230(5) 0.0380(7) -0.0029(4) 0.0283(6) -0.0019(4)
C1 0.0359(7) 0.0276(6) 0.0564(9) -0.0082(5) 0.0335(7) -0.0047(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C1 Rh1 C2 90.08(7)
C1 Rh1 N1 177.89(5)
C2 Rh1 N1 90.79(5)
C1 Rh1 Cl1 89.02(6)
C2 Rh1 Cl1 177.45(4)
N1 Rh1 Cl1 90.20(3)
C5 N1 N2 105.19(11)
C5 N1 Rh1 132.47(9)
N2 N1 Rh1 122.34(8)
C3 N2 N1 111.72(11)
C3 N2 H2A 130.5(10)
N1 N2 H2A 117.6(10)
N1 C5 C4 110.65(12)
N1 C5 H5 124.7
C4 C5 H5 124.7
C3 C4 C5 105.18(11)
C3 C4 H4 127.4
C5 C4 H4 127.4
N2 C3 C4 107.26(13)
N2 C3 H3 126.4
C4 C3 H3 126.4
O2 C2 Rh1 178.91(12)
O1 C1 Rh1 177.82(17)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Rh1 C1 1.8468(15)
Rh1 C2 1.8508(14)
Rh1 N1 2.0887(11)
Rh1 Cl1 2.3649(4)
O2 C2 1.1296(18)
O1 C1 1.1295(19)
N1 C5 1.3373(16)
N1 N2 1.3417(14)
N2 C3 1.3386(16)
N2 H2A 0.865(9)
C5 C4 1.388(2)
C5 H5 0.95
C4 C3 1.367(2)
C4 H4 0.95
C3 H3 0.95
