Carboxylate-Based Molybdenum Alkylidene Catalysts: Synthesis, Characterization, and Use as Initiators for 1,6-Heptadiyne Cyclopolymerizations
Schrock, Richard R.; Tonzetich, Zachary J.; Lichtscheidl, Alejandro G.; Müller, Peter; Schattenmann, Florian J.; Organometallics 27 (2008) 3986–; doi:10.1021/om800314y

data_4071684
_publ_section_title
;
 Carboxylate-Based Molybdenum Alkylidene Catalysts: Synthesis,
 Characterization, and Use as Initiators for 1,6-Heptadiyne
 Cyclopolymerizations
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              3986
_journal_paper_doi               10.1021/om800314y
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C66.5 H82 Cl2 Mo N O4 P'
_chemical_formula_weight         1157.14
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                81.6190(10)
_cell_angle_beta                 77.5020(10)
_cell_angle_gamma                88.9480(10)
_cell_formula_units_Z            2
_cell_length_a                   12.7389(3)
_cell_length_b                   14.0067(4)
_cell_length_c                   17.7003(4)
_cell_measurement_reflns_used    9564
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.54
_cell_measurement_theta_min      2.38
_cell_volume                     3050.21(13)
_computing_cell_refinement       'SAINT 5 (Bruker-AXS, 2003)'
_computing_data_collection       'SMART 5 (Bruker-AXS, 2003)'
_computing_data_reduction        'SAINT 5 (Bruker-AXS, 2003)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       'omega and phi scans'
_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  0.0259
_diffrn_reflns_av_sigmaI/netI    0.0222
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            68763
_diffrn_reflns_theta_full        29.57
_diffrn_reflns_theta_max         29.57
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    0.376
_exptl_absorpt_correction_T_max  0.9286
_exptl_absorpt_correction_T_min  0.9119
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1222
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.425
_refine_diff_density_min         -1.172
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     717
_refine_ls_number_reflns         17080
_refine_ls_number_restraints     299
_refine_ls_restrained_S_all      1.156
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0390
_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^)+(0.0573P)^2^+2.8767P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1040
_refine_ls_wR_factor_ref         0.1074
_reflns_number_gt                15509
_reflns_number_total             17080
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800314y-file004.cif
_cod_data_source_block           06052
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C66.50 H82 Cl2 Mo N O4 P'
_cod_database_code               4071684