Reactivity of the Heterometallic Clusters [HMCo3(CO)12] and [Et4N][MCo3(CO)12] (M = Fe, Ru) toward Phosphine Selenides, Including Selenium Transfer. Crystal Structures of [HRuCo3(CO)7(μ-CO)3(μ-dppy)], [MCo2(μ3-Se)(CO)7(μ-dppy)], and [RuCo2(μ3-Se)(CO)7(μ-dppm)] [dppy = Ph2(2-C5H4N)P, dppm = Ph2PCH2PPh2]
Pierre Braunstein; Claudia Graiff; Chiara Massera; Giovanni Predieri; Jacky Rosé; Antonio Tiripicchio; Inorganic Chemistry 41 (2002) 1372–1382; doi:10.1021/ic010824x

data_4317696
_publ_contact_author
;
 Prof. Antonio Tiripicchio
 Dipartimento di Chimica Generale e Inorganica,
 Chimica Analitica, Chimica Fisica,
 Centro di studio per la Strutturistica Diffrattometrica del CNR
 Parco Area delle Scienze 43100 Parma, Italy
;
_publ_contact_author_email       TIRI@IPRUNIV.CCE.UNIPR.IT
_publ_section_title
;
 Reactivity of the Heterometallic Clusters [HMCo3(CO)12] and
 [Et4N][MCo3(CO)12] (M = Fe, Ru) toward Phosphine Selenides, Including
 Selenium Transfer. Crystal Structures of [HRuCo3(CO)7(\m-CO)3(\m-dppy)],
 [MCo2(\m3-Se)(CO)7(\m-dppy)], and [RuCo2(\m3-Se)(CO)7(\m-dppm)] [dppy =
 Ph2(2-C5H4N)P, dppm = Ph2PCH2PPh2]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1372
_journal_page_last               1382
_journal_paper_doi               10.1021/ic010824x
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C27 H15 Co3 N O10 P Ru'
_chemical_formula_weight         822.23
_chemical_name_systematic
;
?
;
_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                 103.47(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.459(4)
_cell_length_b                   11.083(5)
_cell_length_c                   22.472(5)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_volume                     3018(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Philips PW1100'
_diffrn_measurement_method       '\q/2\q 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  0.0617
_diffrn_reflns_av_sigmaI/netI    0.2025
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7449
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         3.34
_diffrn_standards_interval_count 100
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    2.220
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.7318
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            bordeaux
_exptl_crystal_density_diffrn    1.810
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.659
_refine_diff_density_min         -0.408
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.644
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     395
_refine_ls_number_reflns         7281
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.644
_refine_ls_R_factor_all          0.1540
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.321
_refine_ls_shift/su_mean         0.011
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0129P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0538
_refine_ls_wR_factor_ref         0.0796
_reflns_number_gt                2629
_reflns_number_total             7281
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010824x_2.cif
_cod_data_source_block           c9bxf
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0129P)^2^+0.0000P] 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^)+(0.0129P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3017.6(18)
_cod_original_sg_symbol_H-M      'P 1 21/c 1'
_cod_database_code               4317696