#------------------------------------------------------------------------------
#$Date: 2016-03-21 07:40:25 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178576 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/86/4068681.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_4068681
loop_
_publ_author_name
'Fung, Hong Sang'
'Chan, Yun Wai'
'Cheung, Chi Wai'
'Choi, Kwong Shing'
'Lee, Siu Yin'
'Qian, Ying Ying'
'Chan, Kin Shing'
_publ_section_title
;
 Reactivity Studies of Rhodium(III) Porphyrins with Methanol in Alkaline
 Media
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3981
_journal_paper_doi               10.1021/om801029k
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C51 H47 N4 O3 Rh'
_chemical_formula_weight         866.84
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.665(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   28.950(10)
_cell_length_b                   16.893(6)
_cell_length_c                   10.248(4)
_cell_measurement_reflns_used    921
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.56
_cell_measurement_theta_min      2.32
_cell_volume                     4720(3)
_computing_cell_refinement       'BRUKER SMART CCD DIFFRACTOMETER'
_computing_data_collection       'BRUKER SMART CCD DIFFRACTOMETER'
_computing_data_reduction        'BRUKER SMART CCD DIFFRACTOMETER'
_computing_molecular_graphics    'SIEMENS SHELXTL'
_computing_publication_material  'SIEMENS SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'BRUKER SMART CCD DIFFRACTOMETER'
_diffrn_measurement_method       'OMEGA SCAN'
_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  0.0609
_diffrn_reflns_av_sigmaI/netI    0.0746
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            12841
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    0.405
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.416323
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.220
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1800
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.231
_refine_diff_density_min         -0.716
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         4308
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.1392
_refine_ls_R_factor_gt           0.0823
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1919P)²+5.9070P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2462
_refine_ls_wR_factor_ref         0.3164
_reflns_number_gt                2542
_reflns_number_total             4308
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om801029k_si_003.cif
_cod_data_source_block           hsf7.2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        4719(3)
_cod_original_sg_symbol_H-M      C2/m
_cod_database_code               4068681
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'
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 0.58967(3) 0.5000 0.47717(9) 0.0549(4) Uani 1 2 d S
N1 N 0.5895(2) 0.3799(4) 0.4737(6) 0.0561(17) Uani 1 1 d .
N2 N 0.5184(3) 0.5000 0.3578(9) 0.053(2) Uani 1 2 d S
N3 N 0.6583(3) 0.5000 0.6136(10) 0.056(2) Uani 1 2 d S
C1 C 0.6294(3) 0.3324(5) 0.5330(9) 0.061(2) Uani 1 1 d .
C2 C 0.6180(3) 0.2543(6) 0.4786(10) 0.072(3) Uani 1 1 d .
H2A H 0.6388 0.2107 0.5021 0.086 Uiso 1 1 calc R
C3 C 0.5727(3) 0.2547(6) 0.3887(10) 0.070(2) Uani 1 1 d .
H3A H 0.5565 0.2121 0.3354 0.084 Uiso 1 1 calc R
C4 C 0.5529(3) 0.3328(5) 0.3882(9) 0.058(2) Uani 1 1 d .
C5 C 0.5056(3) 0.3570(5) 0.3179(9) 0.060(2) Uani 1 1 d .
C6 C 0.4890(3) 0.4334(5) 0.3132(8) 0.055(2) Uani 1 1 d .
C7 C 0.4389(3) 0.4604(6) 0.2534(9) 0.064(2) Uani 1 1 d .
H7 H 0.4114 0.4281 0.2204 0.077 Uiso 1 1 calc R
C8 C 0.6743(3) 0.6437(5) 0.6321(9) 0.059(2) Uani 1 1 d .
C9 C 0.6864(3) 0.5662(5) 0.6721(9) 0.061(2) Uani 1 1 d .
C10 C 0.7313(3) 0.5406(6) 0.7735(10) 0.072(3) Uani 1 1 d .
H10 H 0.7559 0.5731 0.8294 0.086 Uiso 1 1 calc R
C11 C 0.4693(3) 0.2956(6) 0.2338(10) 0.065(2) Uani 1 1 d .
C12 C 0.4516(4) 0.2360(6) 0.2917(11) 0.078(3) Uani 1 1 d .
H12A H 0.4608 0.2327 0.3877 0.093 Uiso 1 1 calc R
C13 C 0.4205(4) 0.1804(7) 0.2114(14) 0.092(3) Uani 1 1 d .
H13A H 0.4095 0.1398 0.2549 0.110 Uiso 1 1 calc R
C14 C 0.4048(4) 0.1821(8) 0.0707(15) 0.095(4) Uani 1 1 d .
C15 C 0.4227(4) 0.2431(9) 0.0080(12) 0.104(4) Uani 1 1 d .
H15A H 0.4136 0.2458 -0.0880 0.125 Uiso 1 1 calc R
C16 C 0.4541(4) 0.2994(8) 0.0899(11) 0.094(4) Uani 1 1 d .
H16A H 0.4652 0.3405 0.0478 0.112 Uiso 1 1 calc R
C17 C 0.3698(5) 0.1202(8) -0.0159(17) 0.137(6) Uani 1 1 d .
H17A H 0.3618 0.0830 0.0442 0.205 Uiso 1 1 calc R
H17B H 0.3850 0.0928 -0.0729 0.205 Uiso 1 1 calc R
H17C H 0.3403 0.1456 -0.0737 0.205 Uiso 1 1 calc R
C21 C 0.7104(3) 0.7073(5) 0.7005(9) 0.062(2) Uani 1 1 d .
C22 C 0.7022(4) 0.7568(7) 0.7946(12) 0.088(3) Uani 1 1 d .
H22A H 0.6736 0.7514 0.8157 0.106 Uiso 1 1 calc R
C23 C 0.7358(4) 0.8158(7) 0.8606(14) 0.101(4) Uani 1 1 d .
H23A H 0.7287 0.8499 0.9225 0.121 Uiso 1 1 calc R
C24 C 0.7784(4) 0.8238(6) 0.8356(13) 0.083(3) Uani 1 1 d .
C25 C 0.7871(4) 0.7756(7) 0.7417(14) 0.097(4) Uani 1 1 d .
H25A H 0.8160 0.7811 0.7221 0.116 Uiso 1 1 calc R
C26 C 0.7526(4) 0.7165(7) 0.6718(11) 0.087(3) Uani 1 1 d .
H26A H 0.7590 0.6841 0.6065 0.104 Uiso 1 1 calc R
C27 C 0.8169(5) 0.8846(8) 0.9181(15) 0.119(5) Uani 1 1 d .
H27A H 0.8043 0.9133 0.9797 0.179 Uiso 1 1 calc R
H27B H 0.8240 0.9208 0.8551 0.179 Uiso 1 1 calc R
H27C H 0.8464 0.8575 0.9710 0.179 Uiso 1 1 calc R
C31 C 0.6209(5) 0.5000 0.3239(15) 0.090(5) Uani 1 2 d SD
C32 C 0.5581(9) 0.5000 0.089(3) 0.170(11) Uani 1 2 d SD
O1 O 0.5927(6) 0.5380(10) 0.1993(17) 0.114(6) Uani 0.50 1 d PD
O1W O 0.8442(14) 0.5000 0.353(4) 0.35(2) Uani 1 2 d S
O2 O 0.7772(13) 0.5000 0.450(4) 0.40(3) Uani 1 2 d SD
H2 H 0.7700 0.4543 0.4239 0.596 Uiso 0.50 1 calc PR
C41 C 0.8178(14) 0.5000 0.575(3) 0.44(5) Uani 1 2 d SD
H41A H 0.8377 0.5459 0.5779 0.666 Uiso 0.50 1 calc PR
H41B H 0.8370 0.4531 0.5796 0.666 Uiso 0.50 1 calc PR
H41C H 0.8062 0.5010 0.6525 0.666 Uiso 1 2 calc SR
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 0.0000 0.0000 '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 0.0060 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N3 Rh1 N2 173.9(4) . .
N3 Rh1 N1 90.48(16) . 6_565
N2 Rh1 N1 89.61(16) . 6_565
N3 Rh1 N1 90.48(16) . .
N2 Rh1 N1 89.61(16) . .
N1 Rh1 N1 178.1(4) 6_565 .
N3 Rh1 C31 86.9(5) . .
N2 Rh1 C31 99.2(5) . .
N1 Rh1 C31 89.20(18) 6_565 .
N1 Rh1 C31 89.20(18) . .
C1 N1 C4 107.3(7) . .
C1 N1 Rh1 125.5(5) . .
C4 N1 Rh1 125.8(5) . .
C6 N2 C6 107.8(9) 6_565 .
C6 N2 Rh1 126.0(4) 6_565 .
C6 N2 Rh1 126.0(4) . .
C9 N3 C9 106.6(9) . 6_565
C9 N3 Rh1 126.7(5) . .
C9 N3 Rh1 126.7(5) 6_565 .
N1 C1 C8 125.8(8) . 6_565
N1 C1 C2 108.6(7) . .
C8 C1 C2 125.6(8) 6_565 .
C3 C2 C1 108.1(8) . .
C2 C3 C4 107.9(8) . .
N1 C4 C5 125.3(8) . .
N1 C4 C3 107.9(7) . .
C5 C4 C3 126.8(8) . .
C6 C5 C4 124.9(8) . .
C6 C5 C11 117.0(7) . .
C4 C5 C11 118.1(8) . .
C5 C6 N2 125.4(7) . .
C5 C6 C7 127.0(8) . .
N2 C6 C7 107.5(8) . .
C7 C7 C6 108.4(5) 6_565 .
C9 C8 C1 124.5(8) . 6_565
C9 C8 C21 118.2(7) . .
C1 C8 C21 117.3(8) 6_565 .
C8 C9 N3 125.3(7) . .
C8 C9 C10 125.6(8) . .
N3 C9 C10 109.0(8) . .
C10 C10 C9 107.6(5) 6_565 .
C12 C11 C16 117.9(9) . .
C12 C11 C5 123.3(9) . .
C16 C11 C5 118.8(9) . .
C11 C12 C13 121.0(10) . .
C14 C13 C12 122.8(11) . .
C13 C14 C15 117.3(10) . .
C13 C14 C17 121.6(14) . .
C15 C14 C17 121.1(13) . .
C16 C15 C14 119.6(11) . .
C15 C16 C11 121.3(11) . .
C22 C21 C26 118.0(9) . .
C22 C21 C8 120.9(8) . .
C26 C21 C8 121.1(9) . .
C21 C22 C23 121.6(10) . .
C24 C23 C22 120.8(11) . .
C25 C24 C23 118.5(10) . .
C25 C24 C27 121.4(11) . .
C23 C24 C27 120.0(12) . .
C24 C25 C26 121.2(10) . .
C21 C26 C25 120.0(11) . .
O1 C31 O1 53.9(16) 6_565 .
O1 C31 Rh1 114.9(10) 6_565 .
O1 C31 Rh1 114.9(10) . .
O1 C32 O1 55.1(16) . 6_565
O1 O1 C32 62.5(8) 6_565 .
O1 O1 C31 63.0(8) 6_565 .
C32 O1 C31 124.2(16) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Rh1 N3 2.008(9) .
Rh1 N2 2.014(9) .
Rh1 N1 2.030(7) 6_565
Rh1 N1 2.030(7) .
Rh1 C31 2.059(16) .
N1 C1 1.370(10) .
N1 C4 1.377(10) .
N2 C6 1.392(9) 6_565
N2 C6 1.392(9) .
N3 C9 1.395(10) .
N3 C9 1.395(10) 6_565
C1 C8 1.411(11) 6_565
C1 C2 1.426(12) .
C2 C3 1.326(12) .
C3 C4 1.437(13) .
C4 C5 1.378(11) .
C5 C6 1.374(12) .
C5 C11 1.522(12) .
C6 C7 1.443(11) .
C7 C7 1.340(19) 6_565
C8 C9 1.381(12) .
C8 C1 1.411(11) 6_565
C8 C21 1.500(11) .
C9 C10 1.430(12) .
C10 C10 1.371(19) 6_565
C11 C12 1.354(13) .
C11 C16 1.391(13) .
C12 C13 1.367(14) .
C13 C14 1.359(17) .
C14 C15 1.402(19) .
C14 C17 1.518(15) .
C15 C16 1.385(16) .
C21 C22 1.356(14) .
C21 C26 1.359(13) .
C22 C23 1.398(14) .
C23 C24 1.348(15) .
C24 C25 1.346(16) .
C24 C27 1.542(15) .
C25 C26 1.422(15) .
C31 O1 1.416(9) 6_565
C31 O1 1.416(9) .
C32 O1 1.389(10) .
C32 O1 1.389(10) 6_565
O1 O1 1.28(3) 6_565
O2 C41 1.421(10) .
