Isomeric molecular rectangles resulting from self-assembly of dicopper complexes of macrocyclic ligands.
Company, Anna; Gómez, Laura; López Valbuena, Josep Maria; Mas-Ballesté, Ruben; Benet-Buchholz, Jordi; Llobet, Antoni; Costas, Miquel; Inorganic chemistry 45 (2006) 2501–2508; doi:10.1021/ic051759k

data_4340202
_publ_contact_author
;
    Dr. Benet-Buchholz, Jordi
    Institut Catal\`a d'Investigaci\'o Qu\'imica (ICIQ)    
    X-ray Diffraction Unit
    Avgda. Pa\=isos Catalans 16
    E-43007 Tarragona, Spain
;
_publ_section_title
;
 Isomeric molecular rectangles resulting from self-assembly of dicopper
 complexes of macrocyclic ligands.
;
_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2501
_journal_page_last               2508
_journal_paper_doi               10.1021/ic051759k
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C32.5 H46 Cu2 F8 N6 O10 S3.5'
_chemical_formula_weight         1072.04
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           63
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.2529(8)
_cell_length_b                   26.1686(18)
_cell_length_c                   27.4119(16)
_cell_measurement_temperature    153(2)
_cell_volume                     10224.0(11)
_computing_cell_refinement       'Bruker SAINT program Vers. 5.0'
_computing_data_collection       'Bruker SMART CCD area detector system'
_computing_data_reduction        'Bruker SAINT program Vers. 5.0'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 512
_diffrn_detector_type            'Smart 1000 CCD area detector'
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device_type  'four-circle diffractometer Bruker P4'
_diffrn_measurement_method
;
 Fullsphere data collection, phi and omega scans,
 in omega at 0.3 deg scan width, three runs with 98, 67 and 67 frames, phi=0 deg
 in phi at 0.3 deg scan width, two runs with 1207 frames, omega=-32 deg
;
_diffrn_measurement_specimen_support
'magnetic support whith 10 micron nylon fiber cryoloop'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1669
_diffrn_reflns_av_sigmaI/netI    0.1424
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            66074
_diffrn_reflns_theta_full        31.57
_diffrn_reflns_theta_max         31.57
_diffrn_reflns_theta_min         1.63
_diffrn_source                   'rotating anode X-ray tube'
_diffrn_source_current           220
_diffrn_source_power             47
_diffrn_source_size              '10 mm x 0.5 mm fine focus'
_diffrn_source_type              'MACScience Co. M18X-HF'
_exptl_absorpt_coefficient_mu    1.055
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.760220
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 SADABS Version 2.1 2003 Bruker-Nonius
 Blessing, Acta Cryst. (1995) A51 33-38
;
_exptl_crystal_colour            black/red/yellow
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4392
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.047
_refine_diff_density_min         -1.211
_refine_diff_density_rms         0.188
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.920
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     510
_refine_ls_number_reflns         8473
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      0.922
_refine_ls_R_factor_all          0.2295
_refine_ls_R_factor_gt           0.1043
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1762P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2742
_refine_ls_wR_factor_ref         0.3254
_reflns_number_gt                2960
_reflns_number_total             8473
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051759ksi20051011_104311.cif
_cod_data_source_block           jm1p28_1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_diffrn_measurement_specimen_suppport' tag replaced with
'_diffrn_measurement_specimen_support'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      Cmcm
_cod_original_formula_sum        'C32.50 H46 Cu2 F8 N6 O10 S3.50'
_cod_database_code               4340202