Selective hydrosiloxane synthesis via dehydrogenative coupling of silanols with hydrosilanes catalysed by Fe complexes bearing a tetradentate PNNP ligand.
Takeshita, Tomohiro; Sato, Kazuhiko; Nakajima, Yumiko; Dalton transactions (Cambridge, England : 2003) 47 (2018) 17004–17010; doi:10.1039/c8dt04168g

data_7048022
_publ_section_title
;
 Selective hydrosiloxane synthesis via dehydrogenative coupling of
 silanols with hydrosilanes catalysed by Fe complexes bearing a
 tetradentate PNNP ligand.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17004
_journal_page_last               17010
_journal_paper_doi               10.1039/c8dt04168g
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C19 H12 Cl N O'
_chemical_formula_sum            'C19 H12 Cl N O'
_chemical_formula_weight         305.75
_chemical_name_systematic        5-(4-Chlorophenyl)-phenanthredin-6-one
_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   geom
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2018-09-10 deposited with the CCDC.
2018-11-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.941(4)
_cell_angle_gamma                90
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_cell_length_c                   10.5965(5)
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_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      28.50
_cell_measurement_theta_min      2.12
_cell_volume                     1447.38(11)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
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_diffrn_detector                 'image plate (34 cm diameter)'
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_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details      ' 138 frames, detector distance = 80 mm'
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 0.998
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_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7429
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.436
_diffrn_reflns_theta_min         2.120
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_exptl_absorpt_coefficient_mu    0.264
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_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            colourless
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_exptl_crystal_description       needle
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_exptl_crystal_size_max          1.070
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0872
_refine_ls_R_factor_gt           0.0579
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0331P)^2^+1.4963P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1158
_refine_ls_wR_factor_ref         0.1329
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2699
_reflns_number_total             3631
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04168g2.cif
_cod_data_source_block           2a
_cod_depositor_comments
'Adding full bibliography for 7048021--7048028.cif.'
_cod_database_code               7048022
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.765
_shelx_estimated_absorpt_t_max   0.990
_shelx_res_checksum              49706