Synthesis and properties of iron-group hydrido-cyano complexes trans-[MH(CN)(L)2], M = Fe, Ru or Os, L = diphosphine, and their hydrogen, trifluoroboron and triphenylboron isocyanide derivatives of the type trans-[MH(CNH)(L)2]O3SCF3, trans-[MH(CNBX3)(L)2], X = F or Ph, and trans-[M(H2)(CNBF3)(dppp)2]BF4 [dppp = Ph2P(CH2)3PPh2]
Rocchini, Eliana; Rigo, Pierluigi; Mezzetti, Antonio; Stephan, Tim; Morris, Robert H.; Lough, Alan J.; Forde, Cameron E.; Fong, Tina P.; Drouin, Samantha D.; Journal of the Chemical Society, Dalton Transactions  (2000) 3591–; doi:10.1039/b005687l

data_7010076
_publ_section_title
;
 Synthesis and properties of iron-group hydrido-cyano complexes
 trans-[MH(CN)(L)2], M&#x2005;=&#x2005;Fe, Ru or Os,
 L&#x2005;=&#x2005;diphosphine, and their hydrogen, trifluoroboron and
 triphenylboron isocyanide derivatives of the type
 trans-[MH(CNH)(L)2]O3SCF3, trans-[MH(CNBX3)(L)2], X&#x2005;=&#x2005;F
 or Ph, and trans-[M(H2)(CNBF3)(dppp)2]BF4
 [dppp&#x2005;=&#x2005;Ph2P(CH2)3PPh2]
;
_journal_issue                   20
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3591
_journal_paper_doi               10.1039/b005687l
_journal_year                    2000
_chemical_formula_sum            'C54 H50 F3 N O3 P4 Ru S'
_chemical_formula_weight         1074.96
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.73(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.536(4)
_cell_length_b                   17.005(2)
_cell_length_c                   22.280(8)
_cell_measurement_reflns_used    58
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      12.54
_cell_measurement_theta_min      3.14
_cell_volume                     6222(3)
_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  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.840
_diffrn_measured_fraction_theta_max 0.840
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_sigmaI/netI    0.0496
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            9532
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.57
_diffrn_standards_decay_%        7.43
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.433
_exptl_absorpt_correction_T_max  0.8774
_exptl_absorpt_correction_T_min  0.8458
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'SHELXTL (Sheldrick, 1997)'
_exptl_crystal_density_diffrn    1.148
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2208
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.31
_refine_diff_density_max         0.559
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     647
_refine_ls_number_reflns         9202
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0457
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0755P)^2^+3.7660P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1260
_refine_ls_wR_factor_ref         0.1319
_reflns_number_gt                7335
_reflns_number_total             9202
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b005687l.txt
_cod_data_source_block           s9743
_cod_depositor_comments
;
 Removing duplicate rows from the ATOM_TYPE loop.

 Antanas Vaitkus,
 2018-08-07

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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_original_formula_sum        'C54 H2 H48 F3 N O3 P4 Ru S'
_cod_database_code               7010076