Crystallization-Induced Asymmetric Transformations in Crotyl Molybdenum Complexes†
Faller, J. W.; Sarantopoulos, Nikos; Crystal Growth & Design 5 (2005) 2356–; doi:10.1021/cg050152b

data_4505176
_publ_section_title
;
 Crystallization-Induced Asymmetric Transformations in Crotyl Molybdenum
 Complexes&#x2020;
;
_journal_issue                   6
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              2356
_journal_paper_doi               10.1021/cg050152b
_journal_volume                  5
_journal_year                    2005
_chemical_absolute_configuration
;
(S)-crotyl;(A)-molybdenum (S,S-Chiraphos)
;
_chemical_formula_moiety         'C34 H35 Cl Mo O2 P2, C H2 Cl2'
_chemical_formula_sum            'C35 H37 Cl3 Mo O2 P2'
_chemical_formula_weight         753.92
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_cell_angle_alpha                90
_cell_angle_beta                 107.278(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.8187(6)
_cell_length_b                   16.4878(7)
_cell_length_c                   11.0874(7)
_cell_measurement_reflns_used    7027
_cell_measurement_temperature    183.2
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.0
_cell_volume                     1713.93(17)
_computing_cell_refinement       Denzo-SMN
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        Denzo-SMN
_computing_publication_material  'teXsan for Windows v. 1.06 (MSC 1999)'
_computing_structure_refinement  'teXsan for Windows v. 1.06 (MSC 1999)'
_computing_structure_solution
;
SIR92 (Altomare, et. al. 1994)
;
_diffrn_ambient_temperature      183.2
_diffrn_measurement_device       'Nonius Kappa CCD'
_diffrn_measurement_method       \w
_diffrn_orient_matrix_UB_11      0.00000
_diffrn_orient_matrix_UB_12      0.00000
_diffrn_orient_matrix_UB_13      0.00000
_diffrn_orient_matrix_UB_21      0.00000
_diffrn_orient_matrix_UB_22      0.00000
_diffrn_orient_matrix_UB_23      0.00000
_diffrn_orient_matrix_UB_31      0.00000
_diffrn_orient_matrix_UB_32      0.00000
_diffrn_orient_matrix_UB_33      0.00000
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.05213
_diffrn_reflns_av_sigmaI/netI    0.122
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10147
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.24
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.739
_exptl_absorpt_correction_T_max  0.953
_exptl_absorpt_correction_T_min  0.862
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 multi-scan from symmetry-related measurements (Blessing 1995)
SORTAV  R.H Blessing,  Acta Cryst., A51, 33-37 (1995),
        J. Appl. Cryst., 30, 421-426 (1997).
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             772.00
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.59
_refine_diff_density_min         -0.66
_refine_ls_abs_structure_details
;
reference to (S,S)-chiraphos
inversion of coordinates(R =4.36,Rw= 4.69 compared to R =4.23, Rw= 4.50)
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.312
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     387
_refine_ls_number_reflns         4450
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0440
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0004
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00002|Fo|^2^]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0670
_refine_ls_wR_factor_ref         0.0490
_reflns_number_gt                4450
_reflns_number_total             6245
_reflns_threshold_expression     I>3.00\s(I)
_cod_data_source_file            cg050152bsi20050414_032004.cif
_cod_data_source_block           '_2137crotylMo(chiraphos)(C'
_cod_depositor_comments
;
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_cell_volume        1713.9(2)
_cod_original_sg_symbol_H-M      'P 21       '
_cod_original_formula_sum        'C35 H37 Cl3 Mo O2 P2 '
_cod_database_code               4505176