Hydrolysis of Coordinated Diazoalkanes To Yield Side-On 1,2-Diazene Derivatives.
Albertin, Gabriele; Antoniutti, Stefano; Botter, Alessandra; Castro, Jesús; Inorganic chemistry 54 (2015) 2091–; doi:10.1021/ic502963n

data_4342447
_publ_section_title
;
 Hydrolysis of Coordinated Diazoalkanes To Yield Side-On 1,2-Diazene
 Derivatives.
;
_journal_issue                   5
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2091
_journal_paper_doi               10.1021/ic502963n
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C31 H41 N2 O3 P2 Ru, C24 H20 B, C H2 Cl2'
_chemical_formula_sum            'C56 H63 B Cl2 N2 O3 P2 Ru'
_chemical_formula_weight         1056.80
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 102.9579(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9766(5)
_cell_length_b                   18.2347(7)
_cell_length_c                   23.2723(8)
_cell_measurement_reflns_used    9771
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      67.40
_cell_measurement_theta_min      3.49
_cell_volume                     5366.6(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker CCD Smart 6000'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Incoatec Quazar MX multilayer optics'
_diffrn_radiation_source         'Incoatec I\muS microsource'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0538
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            39829
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.686
_diffrn_reflns_theta_min         3.110
_exptl_absorpt_coefficient_mu    4.183
_exptl_absorpt_correction_T_max  0.7530
_exptl_absorpt_correction_T_min  0.5382
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_description       prism
_exptl_crystal_F_000             2200
_exptl_crystal_size_max          0.292
_exptl_crystal_size_mid          0.156
_exptl_crystal_size_min          0.130
_refine_diff_density_max         1.299
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         9475
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0535
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0949P)^2^+2.3807P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1483
_refine_ls_wR_factor_ref         0.1576
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7854
_reflns_number_total             9475
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic502963n_si_001.cif
_cod_data_source_block           md_def_ic3
_cod_depositor_comments          'Adding full bibliography for 4342447.cif.'
_cod_database_code               4342447
_shelx_estimated_absorpt_t_min   0.375
_shelx_estimated_absorpt_t_max   0.612
_shelxl_version_number           2014/6
_shelx_res_checksum              72223
_shelx_hkl_checksum              81598