Heteronuclear Chains of Four Metal Atoms Including One Quadruply Bonded Dimetal Unit. Dichromium and Dimolybdenum Compounds with Appended Copper(I) Atoms
F. Albert Cotton; Carlos A. Murillo; Lindsay E. Roy; Hong-Cai Zhou; Inorganic Chemistry 39 (2000) 1743–1747; doi:10.1021/ic991274u

data_4320879
_publ_section_title
;
 Heteronuclear Chains of Four Metal Atoms Including One Quadruply Bonded
 Dimetal Unit. Dichromium and Dimolybdenum Compounds with Appended
 Copper(I) Atoms
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1743
_journal_page_last               1747
_journal_paper_doi               10.1021/ic991274u
_journal_volume                  39
_journal_year                    2000
_chemical_compound_source        synthesized
_chemical_formula_analytical     'not measured'
_chemical_formula_moiety
'Mo2 Cu2 (C17 H16 N3)4 (Cu Cl2)2(C2H3N).(C2H3N)2'
_chemical_formula_structural     'Mo2 Cu2 (DPhIP)4 (CuCl2)2 (CH3CN).(CH3CN)2'
_chemical_formula_sum            'C74 H73 Cl4 Cu4 Mo2 N15'
_chemical_formula_weight         1760.31
_chemical_melting_point          ?
_chemical_name_common            none
_chemical_name_systematic
;
 Tetrakis(2,6-diphenyliminopiperidinato)acetonitrile
dimolybdenum(II)dicopper(I) bis(dichlorocuperate)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_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
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 100.7800(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.0279(8)
_cell_length_b                   17.4881(8)
_cell_length_c                   24.6718(11)
_cell_measurement_reflns_used    7168
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.6
_cell_measurement_theta_min      2.213
_cell_volume                     7217.3(6)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  ciftab
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Bruker SMART CCD'
_diffrn_measurement_method       'Ellipsoid-mask Fitting'
_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  0.0288
_diffrn_reflns_av_sigmaI/netI    0.0475
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            45977
_diffrn_reflns_theta_max         28.96
_diffrn_reflns_theta_min         1.44
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    1.697
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_type   muti-scan
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       square-block
_exptl_crystal_F_000             3560
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.823
_refine_diff_density_min         -0.636
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.998
_refine_ls_goodness_of_fit_obs   1.091
_refine_ls_hydrogen_treatment    calc
_refine_ls_matrix_type           full
_refine_ls_number_parameters     872
_refine_ls_number_reflns         17482
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.019
_refine_ls_restrained_S_obs      1.091
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_obs          0.0330
_refine_ls_shift/esd_max         0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0447P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0946
_refine_ls_wR_factor_obs         0.0842
_reflns_number_observed          12299
_reflns_number_total             17488
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic991274u_4.cif
_cod_data_source_block           xl_compound_4(CH3CN).2(CH3CN)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_symmetry_cell_setting' value
'Monoclinic' changed to 'monoclinic' according to the built-in table
from CIF Core dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0447P)^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^)+(0.0447P)^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 
;
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               4320879