Variable temperature electrochemistry as a powerful method for conformational investigations on the fluxional organometallic complex Mo(His-Nɛ-C2H4CO2Me)(η-allyl)(CO)2 (His = Nδ, N,O-l-histidinate)
van Staveren, Dave R.; Bothe, Eberhard; Weyhermüller, Thomas; Metzler-Nolte, Nils; Chemical Communications  (2001) 131–; doi:10.1039/b007822k

data_7115098
_publ_section_title
;
 Variable temperature electrochemistry as a powerful method for
 conformational investigations on the fluxional organometallic complex
 Mo(His-N&#x025B;-C2H4CO2Me)(\h-allyl)(CO)2 (His = N\d, N,O-l-histidinate)
;
_journal_issue                   1
_journal_name_full               'Chemical Communications'
_journal_page_first              131
_journal_paper_doi               10.1039/b007822k
_journal_year                    2001
_chemical_formula_structural     '[C15 H19 Mo N3 O6], 2 CH3OH'
_chemical_formula_sum            'C17 H27 Mo N3 O8'
_chemical_formula_weight         497.36
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 101.59(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.0928(14)
_cell_length_b                   7.5347(8)
_cell_length_c                   12.1177(14)
_cell_measurement_reflns_used    5092
_cell_measurement_temperature    100(2)
_cell_volume                     1081.6(2)
_computing_cell_refinement       'Siemens SAINT 5'
_computing_data_collection       'Siemens SAINT 5'
_computing_data_reduction        'Siemens SAINT 5'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measurement_device       'Siemens SMART CCD-Detector'
_diffrn_measurement_method       '\w-scan, 0.3 deg./frame'
_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  0.0509
_diffrn_reflns_av_sigmaI/netI    0.0354
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11346
_diffrn_reflns_theta_max         32.50
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    0.653
_exptl_absorpt_correction_type   'Not measured'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_description       'transparent block'
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.35
_refine_diff_density_max         1.066
_refine_diff_density_min         -0.721
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.030
_refine_ls_goodness_of_fit_obs   1.035
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         4668
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.029
_refine_ls_restrained_S_obs      1.034
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_obs          0.0269
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0379P)^2^+0.5477P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0692
_refine_ls_wR_factor_obs         0.0685
_reflns_number_observed          4539
_reflns_number_total             4668
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b007822k.txt
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0379P)^2^+0.5477P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0379P)^2^+0.5477P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               7115098