Catalytic hydration of cyanamides with phosphinous acid-based ruthenium(ii) and osmium(ii) complexes: scope and mechanistic insights
González-Fernández, Rebeca; Álvarez, Daniel; Crochet, Pascale; Cadierno, Victorio; Menéndez, M. Isabel; López, Ramón; Catalysis Science & Technology 10 (2020) 4084–4098; doi:10.1039/D0CY00523A

data_1558164
_publ_section_title
;
 Catalytic hydration of cyanamides with phosphinous acid-based
 ruthenium(ii) and osmium(ii) complexes: scope and mechanistic insights
;
_journal_issue                   12
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              4084
_journal_page_last               4098
_journal_paper_doi               10.1039/D0CY00523A
_journal_volume                  10
_journal_year                    2020
_chemical_formula_moiety         'C16 H29 N2 O1 Cl1 F6 P1 Ru1 Sb1'
_chemical_formula_sum            'C16 H29 Cl F6 N2 O P Ru Sb'
_chemical_formula_weight         668.65
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2020-03-11 deposited with the CCDC.	2020-06-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.1720(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.73940(10)
_cell_length_b                   14.7656(2)
_cell_length_c                   14.6955(2)
_cell_measurement_reflns_used    7972
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      69.4510
_cell_measurement_theta_min      4.2260
_cell_volume                     2420.26(5)
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.2640
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Xcalibur, Onyx, Nova'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12565
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.594
_diffrn_reflns_theta_min         4.232
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    16.067
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.14384
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear intense yellow'
_exptl_crystal_density_diffrn    1.835
_exptl_crystal_description       plate
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.353
_refine_diff_density_min         -0.895
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         4476
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0323
_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^)+(0.0414P)^2^+2.3911P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0782
_refine_ls_wR_factor_ref         0.0816
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4053
_reflns_number_total             4476
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cy00523a2.cif
_cod_data_source_block           5a
_cod_depositor_comments
;Adding full bibliography for 1558164--1558165.cif.

 Adding full bibliography for 1558164--1558165.cif.
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1558164
_shelxl_version_number           2014-3
_shelx_res_checksum              82249