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_7702769
_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 H20 Co Fe Mo O6 P'
_chemical_formula_weight         730.16
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
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_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_cell_angle_beta                 93.51(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.557(4)
_cell_length_b                   20.399(4)
_cell_length_c                   13.625(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
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_cell_measurement_theta_min      17
_cell_volume                     2928.7(13)
_computing_cell_refinement       'standard MSC/Rigaku supplied software'
_computing_data_collection       'standard MSC/Rigaku supplied software'
_computing_data_reduction        'standard MSC/Rigaku supplied software'
_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       AFC5r
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_sigmaI/netI    0.0991
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
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_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
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_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.80
_diffrn_standards_decay_%        0%
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.567
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.871
_exptl_absorpt_correction_type   'empirical (4 psi scans)'
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    1.656
_exptl_crystal_description       prism
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.547
_refine_diff_density_min         -0.521
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
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_refine_ls_goodness_of_fit_obs   1.110
_refine_ls_hydrogen_treatment    constr
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_refine_ls_R_factor_obs          0.0466
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_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0513P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2186
_refine_ls_wR_factor_obs         0.1075
_reflns_number_observed          3252
_reflns_number_total             5152
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b110874n.txt
_cod_data_source_block           mm9633
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

data item '_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0513P)^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^)+(0.0513P)^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      P2(1)/n
_cod_database_code               7702769