Borylation, silylation and selenation of C-H bonds in metal sandwich compounds by applying a directing group strategy
Deb, Mayukh; Singh, Jatinder; Mallik, Shuvadip; Hazra, Susanta; Elias, Anil J.; New J. Chem. 41 (2017) 14528–14538; doi:10.1039/C7NJ02388J

data_7056705
_publ_section_title
;
 Borylation, silylation and selenation of C-H bonds in metal sandwich
 compounds by applying a directing group strategy
;
_journal_issue                   23
_journal_name_full               'New J. Chem.'
_journal_page_first              14528
_journal_page_last               14538
_journal_paper_doi               10.1039/C7NJ02388J
_journal_volume                  41
_journal_year                    2017
_chemical_formula_moiety         'C18 H15 Fe N3 O2 Pd, 0.5(H2 O)'
_chemical_formula_sum            'C18 H16 Fe N3 O2.5 Pd'
_chemical_formula_weight         476.59
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-10-13 deposited with the CCDC.
2017-10-23 downloaded from the CCDC.
;
_cell_angle_alpha                95.62(4)
_cell_angle_beta                 101.53(4)
_cell_angle_gamma                103.73(4)
_cell_formula_units_Z            4
_cell_length_a                   10.80(3)
_cell_length_b                   11.71(3)
_cell_length_c                   15.37(4)
_cell_measurement_reflns_used    3659
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.137
_cell_measurement_theta_min      2.367
_cell_volume                     1828(8)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'Bruker SMART APEX-II'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'DIAMOND 3.2'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2014/5 Bruker-AXS, Madison WI'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1188
_diffrn_reflns_av_unetI/netI     0.1047
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11198
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.303
_diffrn_reflns_theta_min         1.368
_exptl_absorpt_coefficient_mu    1.795
_exptl_absorpt_correction_T_max  0.831
_exptl_absorpt_correction_T_min  0.569
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker; 2014)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.731
_exptl_crystal_description       block
_exptl_crystal_F_000             948
_exptl_crystal_size_max          0.365
_exptl_crystal_size_mid          0.245
_exptl_crystal_size_min          0.115
_refine_diff_density_max         1.113
_refine_diff_density_min         -1.391
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.931
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     465
_refine_ls_number_reflns         8081
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.931
_refine_ls_R_factor_all          0.0816
_refine_ls_R_factor_gt           0.0500
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0650P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1147
_refine_ls_wR_factor_ref         0.1340
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5484
_reflns_number_total             8081
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj02388j2.cif
_cod_data_source_block           2b
_cod_depositor_comments
;

2018-02-14
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        1828(9)
_cod_original_formula_moiety     '2(C18 H15 Fe N3 O2 Pd), H2 O'
_cod_original_formula_sum        'C36 H32 Fe2 N6 O5 Pd2'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     953.18
_cod_database_code               7056705
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.596
_shelx_estimated_absorpt_t_max   0.813
_shelx_res_checksum              33944