Alkylation of Rhodium Porphyrins Using Ammonium and Quinolinium Salts
Thompson, Samuel J.; Dong, Guangbin; Organometallics 33 (2014) 3757–; doi:10.1021/om500438s

data_4083906
_publ_section_title
;
 Alkylation of Rhodium Porphyrins Using Ammonium and Quinolinium Salts
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3757
_journal_paper_doi               10.1021/om500438s
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C44 H28 N4, Rh, C2 H5, 1/2 C Cl4'
_chemical_formula_sum            'C46.5 H33 Cl2 N4 Rh'
_chemical_formula_weight         821.58
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                104.215(2)
_cell_angle_beta                 107.305(2)
_cell_angle_gamma                99.963(2)
_cell_formula_units_Z            2
_cell_length_a                   11.2350(8)
_cell_length_b                   13.1958(10)
_cell_length_c                   13.8948(10)
_cell_measurement_reflns_used    6032
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.6
_cell_volume                     1837.9(2)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_publication_material  'XP SHELXTL/PC, Siemens Analytical'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution
;

Superflip.  Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst. 40, 786-790.
 
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Rigaku AFC-12 with Saturn 724+ CCD'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0749
_diffrn_reflns_av_unetI/netI     0.0875
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24233
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         3.133
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.651
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.592
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Abscor. T. Higashi (2001). The Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_description       prism
_exptl_crystal_F_000             838
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.734
_refine_diff_density_min         -1.048
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         8272
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0825
_refine_ls_R_factor_gt           0.0597
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+6.5834P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1084
_refine_ls_wR_factor_ref         0.1178
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6585
_reflns_number_total             8272
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500438s_si_001.cif
_cod_data_source_block           935
_cod_depositor_comments
'Adding full bibliography for 4083903--4083907.cif.'
_cod_original_formula_sum        'C46.50 H33 Cl2 N4 Rh'
_cod_database_code               4083906
_shelx_estimated_absorpt_t_min   0.944
_shelx_estimated_absorpt_t_max   0.968
_shelxl_version_number           2013-4
_shelx_res_checksum              46412
_shelx_hkl_checksum              9125