Electrophilic O-Methylation of a Terminal Nitrosyl Ligand Attained by an Early−Late Heterobimetallic Effect
Arashiba, Kazuya; Matsukawa, Shoji; Kuwata, Shigeki; Tanabe, Yoshiaki; Iwasaki, Masakazu; Ishii, Youichi; Organometallics 25 (2006) 560–; doi:10.1021/om0510573

data_4074955
_publ_section_title
;
 Electrophilic O-Methylation of a Terminal Nitrosyl Ligand Attained by an
 Early&#x2212;Late Heterobimetallic Effect
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              560
_journal_paper_doi               10.1021/om0510573
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety         'C23 H39 N O P Rh S2 W '
_chemical_formula_sum            'C23 H39 N O P Rh S2 W'
_chemical_formula_weight         727.42
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90
_cell_angle_beta                 97.121(8)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.008(2)
_cell_length_b                   18.843(2)
_cell_length_c                   17.127(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293.1
_cell_measurement_theta_max      20.0
_cell_measurement_theta_min      18.7
_cell_volume                     5446.6(11)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.6.0'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    'DIRDIF99 (PATTY)'
_diffrn_measured_fraction_theta_full 0.9989
_diffrn_measured_fraction_theta_max 0.9989
_diffrn_measurement_device_type  'Rigaku AFC7S'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            13308
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_standards_decay_%        -0.38
_diffrn_standards_interval_count 0
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.057
_exptl_absorpt_correction_T_max  0.219
_exptl_absorpt_correction_T_min  0.164
_exptl_absorpt_correction_type   psi-scans
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.774
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2864.00
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.81
_refine_diff_density_min         -1.60
_refine_ls_extinction_coef       32(5)
_refine_ls_extinction_method
'Larson (1970) Crystallographic Computing eq. 22'
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     620
_refine_ls_number_reflns         8566
_refine_ls_R_factor_gt           0.0370
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
'w = 1/[0.0001Fo^2^ + 1.2000\s(Fo^2^) + 0.2500]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0380
_reflns_number_gt                8566
_reflns_number_total             12486
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om0510573si20051210_040451.cif
_cod_data_source_block           '_[Cp*Rh(PMe3)(m-S)2W(NO)Cp*]'
_cod_original_cell_volume        5446(1)
_cod_original_formula_sum        'C23 H39 N O P Rh S2 W '
_cod_database_code               4074955