A reductive recycle strategy for the facile synthesis of molybdenum(VI) alkylidyne catalysts for alkyne metathesis
Zhang, Wei; Kraft, Stefan; Moore, Jeffrey S.; Chemical Communications (Cambridge, United Kingdom)  (2003) 832–833; doi:10.1039/b212405j

data_7104041
_publ_section_title
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 A reductive recycle strategy for the facile synthesis of molybdenum(VI)
 alkylidyne catalysts for alkyne metathesis
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_journal_coden_ASTM              CHCOFS
_journal_issue                   7
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              832
_journal_page_last               833
_journal_paper_doi               10.1039/b212405j
_journal_year                    2003
_chemical_formula_moiety         'C39 H59 Mo N3'
_chemical_formula_sum            'C39 H59 Mo N3'
_chemical_formula_weight         665.83
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
; 
2002-10-22   text and data added, srw & wz 
;
_cell_angle_alpha                90.00
_cell_angle_beta                 104.075(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.144(10)
_cell_length_b                   10.513(6)
_cell_length_c                   19.324(11)
_cell_measurement_reflns_used    1015
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.9
_cell_volume                     3772(4)
_computing_cell_refinement       'SAINT V6 (Bruker, 2001)'
_computing_data_collection       'SMART V5 (Bruker, 2001)'
_computing_data_reduction        'SAINT V6 (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL V6 (Bruker, 2001)'
_computing_publication_material  'CIFTAB (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXTL V6 (Bruker, 2001)'
_computing_structure_solution    'SHELXTL V6 (Bruker, 2001)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Siemens Platform/CCD'
_diffrn_measurement_method       'profile data from \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  p91tas
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_sigmaI/netI    0.0307
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            39471
_diffrn_reflns_theta_full        25.36
_diffrn_reflns_theta_max         25.36
_diffrn_reflns_theta_min         2.17
_diffrn_standards_decay_%        1.6
_diffrn_standards_interval_time  458
_diffrn_standards_number         381
_exptl_absorpt_coefficient_mu    0.376
_exptl_absorpt_correction_T_max  0.9809
_exptl_absorpt_correction_T_min  0.7692
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(Bruker, 2001)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_density_meas      ?
_exptl_crystal_description       platy
_exptl_crystal_F_000             1424
_exptl_crystal_id                p91tas
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.4 mm cryo-loop (Hampton Research) with the (1 1 -1) scattering planes 
roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.59
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.459
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         6919
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0327
_refine_ls_shift/su_max          0.032
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0392P)^2^+2.3444P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0792
_refine_ls_wR_factor_ref         0.0844
_reflns_number_gt                5701
_reflns_number_total             6919
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b212405j.txt
_cod_data_source_block           p91tas
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_Hall     '-P 2ybc '
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_database_code               7104041