Coordination Chemistry of a Model for the GP Cofactor in the Hmd Hydrogenase: Hydrogen-Bonding and Hydrogen-Transfer Catalysis
Aaron M. Royer; Thomas B. Rauchfuss; Scott R. Wilson; Inorganic Chemistry 47 (2008) 395–397; doi:10.1021/ic7018692

data_4304370
_publ_contact_author
; 
Scott R. Wilson 
University of Illinois 
School of Chemical Sciences, Box 59-1 
505 South Mathews Avenue 
Urbana, Illinois  61801 
USA 
;
_publ_contact_author_email       srwilson@uiuc.edu
_publ_contact_author_fax         '1  217 244 8068'
_publ_contact_author_phone       '1  217 244 1708'
_publ_section_title
;
Coordination Chemistry of a Model for the GP Cofactor in the Hmd
Hydrogenase: Hydrogen-Bonding and Hydrogen-Transfer Catalysis
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              395
_journal_page_last               397
_journal_paper_doi               10.1021/ic7018692
_journal_volume                  47
_journal_year                    2008
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C23 H27 N2 O4 Rh, 1.5(C2 H3 N)'
_chemical_formula_sum            'C26 H31.5 N3.5 O4 Rh'
_chemical_formula_weight         559.95
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'I -2ya'
_symmetry_space_group_name_H-M   'I 1 a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
; 
2007-06-29   text and data added, amr 
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.026(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   37.3616(19)
_cell_length_b                   7.3406(4)
_cell_length_c                   37.814(2)
_cell_measurement_reflns_used    9654
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.27
_cell_measurement_theta_min      2.41
_cell_volume                     10370.7(9)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V1.0-27 (Bruker, 2004)'
_computing_data_reduction
'SAINT V7.23A, XPREP V2005/2, SADABS V2007/4 (Bruker, 2005 & 2007)'
_computing_molecular_graphics    'SHELXTL V6.12 (Bruker, 2005)'
_computing_publication_material  'XCIF V6.12 (Bruker, 2005)'
_computing_structure_refinement  'SHELXTL V6.12 (Bruker, 2005)'
_computing_structure_solution    'SHELXTL V6.12 (Bruker, 2005)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device       'Bruker Kappa/ApexII CCD'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  ga59ra
_diffrn_reflns_av_R_equivalents  0.0698
_diffrn_reflns_av_sigmaI/netI    0.0641
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            61924
_diffrn_reflns_theta_full        26.27
_diffrn_reflns_theta_max         26.27
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    0.695
_exptl_absorpt_correction_T_max  0.9209
_exptl_absorpt_correction_T_min  0.8063
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP (Bruker, 2001)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       columnar
_exptl_crystal_F_000             4624
_exptl_crystal_id                ga59ra
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (-1 5 -8) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.950
_refine_diff_density_min         -1.855
_refine_diff_density_rms         0.155
_refine_ls_abs_structure_details 'Flack (1983),  7628 Friedels'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1220
_refine_ls_number_reflns         17651
_refine_ls_number_restraints     2778
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0972
_refine_ls_R_factor_gt           0.0859
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0720P)^2^+376.1533P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2085
_refine_ls_wR_factor_ref         0.2185
_reflns_number_gt                15263
_reflns_number_total             17651
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic7018692-file001.cif
_cod_data_source_block           ga59ra
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

2020-09-09
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C52 H63 N7 O8 Rh2'
_cod_original_formula_weight         1119.91
_cod_original_formula_moiety         '2(C23 H27 N2 O4 Rh), 3(C2 H3 N)'
_cod_original_formula_units_Z            8
_cod_original_cell_volume        10370.8(9)
_cod_original_sg_symbol_Hall     'I -2ya '
_cod_original_sg_symbol_H-M      'I a '
_cod_database_code               4304370