Dynamic Behavior, Redistribution Reactions, and Intermetallic Distances of Dinuclear Bis(μ-pyrazolato)rhodium(I) Complexes
Tejel, Cristina; Villoro, José M.; Ciriano, Miguel A.; López, José A.; Eguizábal, Eduardo; Lahoz, Fernando J.; Bakhmutov, Vladimir I.; Oro, Luis A.; Organometallics 15 (1996) 2967–; doi:10.1021/om960005y

data_4078330
_publ_section_title
;
 Dynamic Behavior, Redistribution Reactions, and Intermetallic Distances
 of Dinuclear Bis(\m-pyrazolato)rhodium(I) Complexes
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              2967
_journal_paper_doi               10.1021/om960005y
_journal_volume                  15
_journal_year                    1996
_chemical_formula_structural     '[Rh~2~(\m-pz)~2~(COD)(CN^t^But)~2~]'
_chemical_formula_sum            'C24 H36 N6 Rh2'
_chemical_formula_weight         614.41
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 97.760(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.367(3)
_cell_length_b                   9.993(2)
_cell_length_c                   16.344(3)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.5
_cell_measurement_theta_min      10
_cell_volume                     2810.5(9)
_computing_cell_refinement       'DIF4 (Stoe)'
_computing_data_collection       'DIF4 (Stoe)'
_computing_data_reduction        'REDU4 (Stoe)'
_computing_molecular_graphics    'SHELXTL-PLUS v.4.2 (Siemens)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SIR92 (Giacovazzo, 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens-Stoe AED-2'
_diffrn_measurement_method       '\w/2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal focus Siemens Mo sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0626
_diffrn_reflns_av_sigmaI/netI    0.1253
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            6661
_diffrn_reflns_theta_max         24.96
_diffrn_reflns_theta_min         2.36
_diffrn_standards_decay_%        0.6
_diffrn_standards_interval_time  55
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.195
_exptl_absorpt_correction_T_max  0.690
_exptl_absorpt_correction_T_min  0.554
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_description       'prismatic block'
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.743
_refine_diff_density_min         -0.506
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.009
_refine_ls_goodness_of_fit_obs   1.121
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         4924
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      1.031
_refine_ls_restrained_S_obs      1.134
_refine_ls_R_factor_all          0.1529
_refine_ls_R_factor_obs          0.0565
_refine_ls_shift/esd_max         0.008
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0618P)^2^+2.0422P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1458
_refine_ls_wR_factor_obs         0.1116
_reflns_number_observed          2527
_reflns_number_total             4926
_reflns_observed_criterion       I>2sigma(I)
_cod_data_source_file            om2967.cif
_cod_data_source_block           comp8
_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_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0618P)^2^+2.0422P] 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^)+(0.0618P)^2^+2.0422P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4078330
_atom_sites_solution_hydrogens_special_details
;
 Most of the hydrogen atoms were located in a difference Fourier map, but
 some of them were introduced in calculated positions.
;
_refine_ls_hydrogen_treatment_special_details
;
 The hydrogen atoms were refined riding on the carbon atoms, with two
 free common isotropic thermal parameters.
;