Synthesis and reactions of the cyclooctadienylmolybdenum complexes [MoBr(CO)2(NCMe)2(η3-C8H11)] (η3-C8H11= 1‒3-η:4,5-C8H11 or 1‒3-η:5,6-C8H11)
Dale M. Spencer; Roy L. Beddoes; Rasika K. Dissanayake; Madeleine Helliwell; Mark W. Whiteley; J. Chem. Soc., Dalton Trans.  (2002) 1009–1019; doi:10.1039/b107581k

data_7011101
_publ_section_title
;
 Synthesis and reactions of the cyclooctadienylmolybdenum complexes
 [MoBr(CO)2(NCMe)2(\h3-C8H11)] (\h3-C8H11= 1--3-\h:4,5-C8H11 or
 1--3-\h:5,6-C8H11)
;
_journal_issue                   6
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              1009
_journal_page_last               1019
_journal_paper_doi               10.1039/b107581k
_journal_year                    2002
_chemical_formula_sum            'C20 H19 Br Mo N2 O2'
_chemical_formula_weight         495.23
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_audit_creation_date             19100-09-06
_audit_creation_method           'by teXsan v1.7'
_audit_update_record             ?
_cell_angle_alpha                90
_cell_angle_beta                 112.93(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   35.585(5)
_cell_length_b                   8.05(1)
_cell_length_c                   14.512(3)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      15.2
_cell_volume                     3829(5)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan (MSC, 1995)'
_computing_publication_material  'teXsan (MSC, 1995)'
_computing_structure_refinement  'teXsan (MSC, 1995)'
_computing_structure_solution
;
SIR92 (Altomare, et. al. 1993)
;
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device       'Rigaku AFC5R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.01813
_diffrn_orient_matrix_UB_12      0.05805
_diffrn_orient_matrix_UB_13      0.06242
_diffrn_orient_matrix_UB_21      -0.02454
_diffrn_orient_matrix_UB_22      0.04380
_diffrn_orient_matrix_UB_23      0.00952
_diffrn_orient_matrix_UB_31      -0.00022
_diffrn_orient_matrix_UB_32      -0.10068
_diffrn_orient_matrix_UB_33      0.04014
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.04939
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3138
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         60.17
_diffrn_reflns_theta_min         0.00
_diffrn_standards_decay_%        6.04
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    8.316
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.427
_exptl_absorpt_correction_type
;
\y scans (North,Phillips & Matthews, 1968)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.718
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1968.00
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.82
_refine_diff_density_min         -1.17
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   2.260
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     235
_refine_ls_number_reflns         2193
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0568
_refine_ls_shift/esd_max         0.0010
_refine_ls_shift/esd_mean        0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00022|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0708
_reflns_number_observed          2193
_reflns_number_total             3078
_reflns_observed_criterion       >3.00\s(I)
_cod_data_source_file            b107581k.txt
_cod_data_source_block           s455
_cod_depositor_comments
;
 Homogenising atom site labels in order to relate data from different loops.

 Antanas Vaitkus,
 2018-08-08

 Correcting the data name order in the GEOM_TORSION loop.

 Antanas Vaitkus,
 2018-08-08

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 1/[\s^2^(Fo) +
0.00022|Fo|^2^]' 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) + 0.00022|Fo|^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'C 2/c      '
_cod_original_formula_sum        'C20 H19 Br N2 Mo O2 '
_cod_database_code               7011101