Perpendicular to parallel reorientation of a terminal alkyne on a mixed-metal triangle; synthesis and structural characterisation
Mays, Martin J.; Raithby, Paul R.; Sarveswaran, Koshala; Solan, Gregory A.; Journal of the Chemical Society, Dalton Transactions  (2002) 1671–; doi:10.1039/b110874n

data_7702766
_publ_section_title
;
 Perpendicular to parallel reorientation of a terminal alkyne on a
 mixed-metal triangle; synthesis and structural characterisation
;
_journal_issue                   8
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1671
_journal_paper_doi               10.1039/b110874n
_journal_year                    2002
_chemical_formula_sum            'C31 H21 Fe2 Mo O6 P'
_chemical_formula_weight         728.09
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        '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
_cell_angle_alpha                100.85(2)
_cell_angle_beta                 111.250(10)
_cell_angle_gamma                74.77(2)
_cell_formula_units_Z            2
_cell_length_a                   11.108(2)
_cell_length_b                   13.177(3)
_cell_length_c                   10.810(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      1
_cell_volume                     1415.3(5)
_computing_cell_refinement       'standard MSC/Rigaku supplied software'
_computing_data_collection       'standard MSC/Rigaku supplied software'
_computing_data_reduction        'MSC teXsan'
_computing_molecular_graphics    XP
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Rigaku AFC5-R'
_diffrn_measurement_method       'omega-2theta 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  0.0294
_diffrn_reflns_av_sigmaI/netI    0.0707
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5255
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.72
_diffrn_standards_decay_%        4
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.548
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.863
_exptl_absorpt_correction_type   'empirical (10 psi scans)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.709
_exptl_crystal_description       block
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.624
_refine_diff_density_min         -0.385
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.884
_refine_ls_goodness_of_fit_obs   0.829
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         4964
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_restrained_S_obs      0.829
_refine_ls_R_factor_all          0.0798
_refine_ls_R_factor_obs          0.0380
_refine_ls_shift/esd_max         0.121
_refine_ls_shift/esd_mean        0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1566
_refine_ls_wR_factor_obs         0.1076
_reflns_number_observed          3610
_reflns_number_total             4973
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b110874n.txt
_cod_data_source_block           mm9605
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. A new data item '_refine_ls_weighting_details' was
created with the value set to
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7702766