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_7031978
_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         'C17 H24 Cl Ir N O ,Sb F6'
_chemical_formula_sum            'C17 H24 Cl F6 Ir N O Sb'
_chemical_formula_weight         721.77
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.000(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   8.0156(4)
_cell_length_b                   12.8917(7)
_cell_length_c                   20.3840(10)
_cell_measurement_reflns_used    5866
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.08
_cell_measurement_theta_min      2.55
_cell_volume                     2106.37(19)
_computing_cell_refinement       'SAINT+ v. 6.45 (Bruker AXS, 2003)'
_computing_data_collection       'SMART v. 5.611 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+ v. 6.45 (Bruker AXS, 2003)'
_computing_molecular_graphics    'XP program, SHELXTL v6.12, Bruker2000'
_computing_publication_material  'XCIF program, SHELXTLv6.12, 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 0.976
_diffrn_measured_fraction_theta_max 0.976
_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  0.1301
_diffrn_reflns_av_sigmaI/netI    0.0883
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            21576
_diffrn_reflns_theta_full        28.60
_diffrn_reflns_theta_max         28.60
_diffrn_reflns_theta_min         1.87
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    7.780
_exptl_absorpt_correction_T_max  0.6448
_exptl_absorpt_correction_T_min  0.4804
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Absorption correction based on crystal faces indexing has
been processed with SADABS program.
SADABS: Area-Detector Absorption Correction. (1996)  Bruker-AXS 
 within SAINT+ package, v. 6.45.  
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.276
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             1360
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2'
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.062
_refine_diff_density_max         2.674
_refine_diff_density_min         -3.204
_refine_diff_density_rms         0.271
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.049(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.172
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         5160
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.171
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0663
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+27.3967P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1246
_refine_ls_wR_factor_ref         0.1282
_reflns_number_gt                4668
_reflns_number_total             5160
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt02171a1.cif
_cod_data_source_block           cmpnd_3b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               7031978