Hydroxymethylpyridine containing half-sandwich complexes of Rh(iii), Ir(iii) or Ru(ii).
Carmona, Daniel; Lamata, Pilar; Sánchez, Antonio; Pardo, Pilar; Rodríguez, Ricardo; Ramírez, Paola; Lahoz, Fernando J.; García-Orduña, Pilar; Oro, Luis A.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 15546–15559; doi:10.1039/c4dt02171a

data_7031979
_publ_section_title
;
 Hydroxymethylpyridine containing half-sandwich complexes of Rh(iii),
 Ir(iii) or Ru(ii).
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15546
_journal_page_last               15559
_journal_paper_doi               10.1039/c4dt02171a
_journal_volume                  43
_journal_year                    2014
_chemical_absolute_configuration rmad
_chemical_compound_source        'Synthesis in the lab'
_chemical_formula_moiety         'C38 H39 N2 O3 P Rh, 2(F6 Sb)'
_chemical_formula_sum            'C38 H39 F12 N2 O3 P Rh Sb2'
_chemical_formula_weight         1177.09
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 124.2590(10)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            8
_cell_length_a                   32.966(2)
_cell_length_b                   12.6937(8)
_cell_length_c                   23.6444(15)
_cell_measurement_reflns_used    48455
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.2
_cell_measurement_theta_min      1.25
_cell_volume                     8177.6(9)
_computing_cell_refinement       'SAINT+ v. 5.65 (Bruker AXS, 2003)'
_computing_data_collection       'SMART v. 5.611 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+ v. 5.65 (Bruker AXS, 2003)'
_computing_molecular_graphics    'XP program, SHELXTL v.6.12, Bruker2000'
_computing_publication_material  'XCIF program, SHELXTL v 6.12, BrukerAXS'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1124
_diffrn_reflns_av_sigmaI/netI    0.1572
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            48455
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.20
_diffrn_reflns_theta_min         1.25
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.845
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.739
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS: Area-Detector Absorption Correction (1996) Bruker-AXS
 within SAINT+ package, v. 6.45.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.912
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4600
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane / hexane'
_exptl_crystal_size_max          0.095
_exptl_crystal_size_mid          0.057
_exptl_crystal_size_min          0.056
_refine_diff_density_max         4.439
_refine_diff_density_min         -1.340
_refine_diff_density_rms         0.200
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     671
_refine_ls_number_reflns         17876
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.1264
_refine_ls_R_factor_gt           0.0736
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0627P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1367
_refine_ls_wR_factor_ref         0.1574
_reflns_number_gt                11574
_reflns_number_total             17876
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt02171a1.cif
_cod_data_source_block           cmpnd_4a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 7031976--7031980.cif.
;
_cod_original_cell_volume        8177.5(9)
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               7031979