Orotate complexes of rhodium(I) and iridium(I): effect of coligand, counter ion, and solvent of crystallisation on association via complementary hydrogen bonding
James, Stuart L.; Mingos, D. Michael P.; Xu, Xingling; White, Andrew J. P.; Williams, David J.; Journal of the Chemical Society, Dalton Transactions  (1998) 1335–; doi:10.1039/a708205c

data_7027958
_publ_section_title
;
 Orotate complexes of rhodium(I) and iridium(I): effect of coligand,
 counter ion, and solvent of crystallisation on association via
 complementary hydrogen bonding
;
_journal_issue                   8
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1335
_journal_paper_doi               10.1039/a708205c
_journal_year                    1998
_chemical_formula_sum            'C20 H32 Cl2 Ir N3 O4'
_chemical_formula_weight         641.59
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 96.832(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.9618(10)
_cell_length_b                   9.8810(2)
_cell_length_c                   29.6845(11)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      27.98
_cell_measurement_theta_min      11.20
_cell_volume                     4648.6(4)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_av_sigmaI/netI    0.0384
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            3795
_diffrn_reflns_theta_max         61.99
_diffrn_reflns_theta_min         3.00
_diffrn_standards_decay_%        10.45
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    13.498
_exptl_absorpt_correction_T_max  0.2200
_exptl_absorpt_correction_T_min  0.0868
_exptl_absorpt_correction_type   Semi-empirical
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.833
_exptl_crystal_description       Prisms
_exptl_crystal_F_000             2528
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.065
_refine_diff_density_min         -0.897
_refine_diff_density_rms         0.146
_refine_ls_extinction_coef       0.00009(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.046
_refine_ls_goodness_of_fit_obs   1.071
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         3634
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.067
_refine_ls_restrained_S_obs      1.069
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_obs          0.0419
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0679P)^2^+10.0693P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1136
_refine_ls_wR_factor_obs         0.1040
_reflns_number_observed          3063
_reflns_number_total             3649
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            c708205sup1.cif
_cod_data_source_block           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 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0679P)^2^+10.0693P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0679P)^2^+10.0693P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C20 H32 N3 O4 Cl2 Ir'
_cod_database_code               7027958