Synthesis and characterisation of [(triphos)Fe(CO)H2] and its protonation to a dihydrogen complex via an unconventional hydrogen-bonded intermediate
Guilera, Gemma; McGrady, G. Sean; Steed, Jonathan W.; Burchell, Richard P. L.; Sirsch, Peter; Deeming, Anthony J.; New Journal of Chemistry 32 (2008) 1573–; doi:10.1039/b801652f

data_7051964
_publ_section_title
;
 Synthesis and characterisation of [(triphos)Fe(CO)H2] and its
 protonation to a dihydrogen complex via an unconventional
 hydrogen-bonded intermediate
;
_journal_issue                   9
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1573
_journal_paper_doi               10.1039/b801652f
_journal_volume                  32
_journal_year                    2008
_chemical_formula_sum            'C42 H41 Fe O P3'
_chemical_formula_weight         710.51
_chemical_name_common            ggban3
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.489(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.1997(3)
_cell_length_b                   18.1058(6)
_cell_length_c                   18.9884(7)
_cell_measurement_temperature    120(2)
_cell_volume                     3484.2(2)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Hooft, 1999)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'X-Seed (Barbour, 1999)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1198
_diffrn_reflns_av_sigmaI/netI    0.1477
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            17650
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.00
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    0.604
_exptl_absorpt_correction_T_max  0.8637
_exptl_absorpt_correction_T_min  0.8396
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.721
_refine_diff_density_min         -0.612
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       0.0016(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         5907
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1250
_refine_ls_R_factor_gt           0.0588
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0157P)^2^+3.4534P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0869
_refine_ls_wR_factor_ref         0.1057
_reflns_number_gt                3612
_reflns_number_total             5907
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b801652f.txt
_cod_data_source_block           C:\structs\AGemma\ggban3\GGBAN3.CIF
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7051964