Short Intramolecular N-H...C(carbonyl) Interactions in Mixed-Ligand Molybdenum Hexacarbonyl Derivatives
Budge, Matthew G.; Muir, Kathleen J.; McQuillan, Geoffrey P.; Harrison, William T.A.; Crystals 1 (2012) 47–58; doi:10.3390/cryst1020047

data_1508403
_publ_section_title
;
 Short Intramolecular N-H...C(carbonyl) Interactions in Mixed-Ligand
 Molybdenum Hexacarbonyl Derivatives
;
_journal_issue                   2
_journal_name_full               Crystals
_journal_page_first              47
_journal_page_last               58
_journal_paper_doi               10.3390/cryst1020047
_journal_volume                  1
_journal_year                    2012
_chemical_formula_moiety         'C25 H17 Mo N5 O3'
_chemical_formula_sum            'C25 H17 Mo N5 O3'
_chemical_formula_weight         531.38
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.324(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.0965(5)
_cell_length_b                   13.0586(6)
_cell_length_c                   16.6135(8)
_cell_measurement_reflns_used    4539
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.74
_cell_measurement_theta_min      2.48
_cell_volume                     2285.31(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker SMART1000 CCD'
_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  0.0396
_diffrn_reflns_av_sigmaI/netI    0.0600
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            19982
_diffrn_reflns_theta_full        30.07
_diffrn_reflns_theta_max         30.07
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    0.611
_exptl_absorpt_correction_T_max  0.925
_exptl_absorpt_correction_T_min  0.877
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS '
_exptl_crystal_colour            'very dark red'
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.415
_refine_diff_density_min         -0.647
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.868
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         6642
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.868
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0349
_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^)+(0.0280P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0622
_refine_ls_wR_factor_ref         0.0700
_reflns_number_gt                4201
_reflns_number_total             6642
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file
C25H17MoN5O3_P21_n_crystals-01-00047-s001_moco1_DC148.CIF
_cod_data_source_block           km07_chateigner_1508403
_cod_depositor_comments          'journal volume and issue reversed'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1508403