Synthesis and characterisation of amino and bromo ring substituted derivatives of [Ru6C(CO)14L] (L = [2.2]paracyclophane)
Schooler, Paul; Johnson, Brian F. G.; Parsons, Simon; Journal of the Chemical Society, Dalton Transactions  (1999) 559–; doi:10.1039/a808886a

data_7027174
_publ_section_title
;
 Synthesis and characterisation of amino and bromo ring substituted
 derivatives of [Ru6C(CO)14L] (L&#x2005;=&#x2005;[2.2]paracyclophane)
;
_journal_issue                   4
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              559
_journal_paper_doi               10.1039/a808886a
_journal_year                    1999
_chemical_formula_moiety         Ru6C(CO)14(C16H15NH2).2.25CH2Cl2
_chemical_formula_sum            'C33.25 H21.5 Cl4.5 N O14 Ru6'
_chemical_formula_weight         1424.96
_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     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                108.10(2)
_cell_angle_beta                 90.18(2)
_cell_angle_gamma                103.26(3)
_cell_formula_units_Z            2
_cell_length_a                   10.500(4)
_cell_length_b                   14.374(5)
_cell_length_c                   15.037(5)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      20
_cell_volume                     2092.9(13)
_computing_cell_refinement       'Stoe DIF4'
_computing_data_collection       'Stoe DIF4'
_computing_data_reduction        'Stoe REDU4'
_computing_molecular_graphics    SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    DIRDIF
_diffrn_ambient_temperature      220(2)
_diffrn_measurement_device
; 
Stoe Stadi-4 diffractometer with 
Oxford Cryosystems variable temperature device. 
;
_diffrn_measurement_method       Omega-theta
_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  0.0630
_diffrn_reflns_av_sigmaI/netI    0.1174
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7889
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.55
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.462
_exptl_absorpt_correction_T_max  0.875
_exptl_absorpt_correction_T_min  0.652
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    2.261
_exptl_crystal_description       lath
_exptl_crystal_F_000             1361
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.596
_refine_diff_density_min         -1.106
_refine_diff_density_rms         0.205
_refine_ls_extinction_coef       0.0002(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.974
_refine_ls_goodness_of_fit_obs   1.073
_refine_ls_hydrogen_treatment    Riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         7367
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.977
_refine_ls_restrained_S_obs      1.073
_refine_ls_R_factor_all          0.1210
_refine_ls_R_factor_obs          0.0594
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0582P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1447
_refine_ls_wR_factor_obs         0.1194
_reflns_number_observed          4355
_reflns_number_total             7377
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            808886asup1.cif
_cod_data_source_block           ac6242
_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 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'Numerical'
changed to 'numerical' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0582P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' 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^2^)+(0.0582P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'Geometric' was changed to
'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        2092.8(13)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C33.25 H21.50 Cl4.50 N O14 Ru6'
_cod_database_code               7027174