Coordination polymers of a dipyridylazacrown ligand: structural, thermal and spectroscopic properties
Gee, William J.; Moubaraki, Boujemaa; Murray, Keith S.; Batten, Stuart R.; CrystEngComm 15 (2013) 9655–; doi:10.1039/c3ce41202d

data_7211077
_publ_section_title
;
 Coordination polymers of a dipyridylazacrown ligand: structural, thermal
 and spectroscopic properties
;
_journal_issue                   45
_journal_name_full               CrystEngComm
_journal_page_first              9655
_journal_paper_doi               10.1039/c3ce41202d
_journal_volume                  15
_journal_year                    2013
_chemical_formula_moiety
'C50 H74 Fe N10 O8 S2, 2(Cl O4), 2(C4 H8 O), 2(H2 O)'
_chemical_formula_sum            'C58 H94 Cl2 Fe N10 O20 S2'
_chemical_formula_weight         1442.30
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   12.6015(3)
_cell_length_b                   23.5649(4)
_cell_length_c                   23.6458(5)
_cell_measurement_reflns_used    9507
_cell_measurement_temperature    123.01(15)
_cell_measurement_theta_max      66.4038
_cell_measurement_theta_min      2.6450
_cell_volume                     7021.7(3)
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_collection       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      123.01(15)
_diffrn_detector_area_resol_mean 10.3389
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega   11.00  108.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       41.0046   57.0000 -120.0000 97

  2 omega  -35.00   52.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       41.0046  -38.0000   90.0000 87

  3 omega   21.00   67.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       92.5000  -92.0000 -170.0000 46

  4 omega   21.00   70.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       92.5000  -45.0000  -60.0000 49

  5 omega   36.00   65.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       92.5000  -30.0000  -60.0000 29

  6 omega   19.00   77.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       92.5000  -45.0000 -150.0000 58

  7 omega   10.00   74.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       92.5000  -95.0000 -120.0000 64

  8 omega   60.00  111.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       92.5000   77.0000 -120.0000 51

  9 omega   18.00   61.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       92.5000  -61.0000 -180.0000 43

 10 omega   30.00   56.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       92.5000 -125.0000 -120.0000 26

 11 omega   71.00   96.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       92.5000 -125.0000 -120.0000 25

 12 omega   30.00   69.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       92.5000  -30.0000  -30.0000 39

 13 omega   17.00   60.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       92.5000  -30.0000    0.0000 43

 14 omega   87.00  130.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       92.5000   61.0000  -60.0000 43

 15 omega  134.00  162.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       92.5000   61.0000  -60.0000 28

 16 omega   82.00  127.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       92.5000  -92.0000 -170.0000 45

 17 omega  133.00  170.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       92.5000   77.0000 -120.0000 37

 18 omega   33.00   65.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       92.5000  -95.0000  120.0000 32

 19 omega   50.00  128.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       92.5000  -86.0000   92.0000 78

 20 omega   78.00  104.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       92.5000  -61.0000 -180.0000 26

 21 omega   12.00   38.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       92.5000  -86.0000   92.0000 26

;
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0422236000
_diffrn_orient_matrix_UB_12      -0.0141584000
_diffrn_orient_matrix_UB_13      0.0594811000
_diffrn_orient_matrix_UB_21      0.1146935000
_diffrn_orient_matrix_UB_22      -0.0067230000
_diffrn_orient_matrix_UB_23      0.0215174000
_diffrn_orient_matrix_UB_31      0.0027476000
_diffrn_orient_matrix_UB_32      0.0634876000
_diffrn_orient_matrix_UB_33      0.0155411000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0809
_diffrn_reflns_av_sigmaI/netI    0.2001
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            43461
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         66.4038
_diffrn_reflns_theta_min         2.6450
_exptl_absorpt_coefficient_mu    3.618
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44283
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             3056.0
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.525
_refine_diff_density_min         -0.548
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         6172
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_gt           0.0503
_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^)+(0.0737P)^2^+3.4584P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1315
_refine_ls_wR_factor_ref         0.1434
_reflns_number_gt                4928
_reflns_number_total             6172
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce41202d.txt
_cod_data_source_block           6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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 
;
_cod_original_cell_volume        7021.7(4)
_cod_database_code               7211077
_cell_oxdiff_length_a            12.6018(4)
_cell_oxdiff_length_b            23.5583(7)
_cell_oxdiff_length_c            23.6520(9)
_cell_oxdiff_angle_alpha         89.998(3)
_cell_oxdiff_angle_beta          89.993(3)
_cell_oxdiff_angle_gamma         90.008(3)
_cell_oxdiff_volume              7021.7(4)
_cell_oxdiff_measurement_reflns_used 9507
_reflns_odcompleteness_completeness 98.48
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1
_chemical_oxdiff_formula         'C20 H20 Fe N6 O6 S2 Cl1'