Extended dipyrrin ligands: candidates for optical metal ion detection under competitive conditions.
Guski, S.; Albrecht, M.; Willms, T.; Albrecht, M.; Nabeshima, T.; Pan, F.; Puttreddy, R.; Rissanen, K.; Chemical communications (Cambridge, England) 53 (2017) 3213–3215; doi:10.1039/c7cc00672a

data_7119729
_publ_section_title
;
 Extended dipyrrin ligands: candidates for optical metal ion detection
 under competitive conditions.
;
_journal_issue                   22
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              3213
_journal_page_last               3215
_journal_paper_doi               10.1039/c7cc00672a
_journal_volume                  53
_journal_year                    2017
_chemical_formula_moiety         'C22 H25 Cl N8 O3 Zn, 0.5(H2 O)'
_chemical_formula_sum            'C22 H26 Cl N8 O3.5 Zn'
_chemical_formula_weight         559.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-12-02
_audit_creation_method
;
Olex2 1.2
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-12-02 deposited with the CCDC.
2017-02-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.268(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   43.6763(10)
_cell_length_b                   14.1945(4)
_cell_length_c                   7.9006(2)
_cell_measurement_reflns_used    10686
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.7420
_cell_measurement_theta_min      2.7360
_cell_volume                     4894.2(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      120
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0107
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -64.00   53.00   1.0000   81.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.5946   19.0000 -180.0000 117

  2 omega  -41.00   49.00   1.0000   81.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.5946   57.0000   30.0000 90

  3 omega  -90.00   10.00   1.0000   81.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.5946  -77.0000    0.0000 100

  4 omega  -20.00   63.00   1.0000   81.0000
omega____ theta____ kappa____ phi______ frames
    -       20.6883  -99.0000  120.0000 83

  5 omega   -1.00   89.00   1.0000   81.0000
omega____ theta____ kappa____ phi______ frames
    -       20.6883   57.0000 -120.0000 90

  6 omega  -20.00   63.00   1.0000   81.0000
omega____ theta____ kappa____ phi______ frames
    -       20.6883  -99.0000  -30.0000 83

  7 omega   -9.00   85.00   1.0000   81.0000
omega____ theta____ kappa____ phi______ frames
    -       20.6883   77.0000  -90.0000 94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0016023000
_diffrn_orient_matrix_UB_12      0.0123697000
_diffrn_orient_matrix_UB_13      -0.0861610000
_diffrn_orient_matrix_UB_21      0.0096980000
_diffrn_orient_matrix_UB_22      -0.0394854000
_diffrn_orient_matrix_UB_23      -0.0107015000
_diffrn_orient_matrix_UB_31      -0.0129413000
_diffrn_orient_matrix_UB_32      -0.0280241000
_diffrn_orient_matrix_UB_33      -0.0231144000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       56
_diffrn_reflns_limit_h_min       -56
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            33084
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.495
_diffrn_reflns_theta_min         1.867
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.157
_exptl_absorpt_correction_T_max  0.189
_exptl_absorpt_correction_T_min  0.060
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_description       block
_exptl_crystal_F_000             2312
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.145
_refine_diff_density_min         -0.761
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         5619
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0928
_refine_ls_R_factor_gt           0.0783
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1421P)^2^+19.4908P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2415
_refine_ls_wR_factor_ref         0.2561
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4389
_reflns_number_total             5619
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc00672a2.cif
_cod_data_source_block           ZnCl_H2O_L1
_cod_depositor_comments
;
          Adding full bibliography for 7119729.cif.

2018-03-04
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C44 H52 Cl2 N16 O7 Zn2'
_cod_original_formula_weight         1118.65
_cod_original_formula_moiety         '2(C22 H25 Cl N8 O3 Zn), H2 O'
_cod_original_formula_units_Z            4
_cod_database_code               7119729
_chemical_oxdiff_formula         'C8 H22 Br2 Au1 Cl4'
_shelx_estimated_absorpt_t_max   0.883
_shelx_estimated_absorpt_t_min   0.753
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H7A,H7B,H7C} of C7, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups, {H9A,H9B,H9C} of C9, {H8C,H8D,H8E} of C8
2. Restrained distances
 O4-H4_$1
 0.88 with sigma of 0.02
3.a Riding coordinates:
 O4(H4)
3.b Rotating group:
 O2(H2A,H2B)
3.c Aromatic/amide H refined with riding coordinates:
 N3(H3), N7(H7), C3(H3A), C5(H5), C12(H12), C13(H13), C15(H15), C18(H18),
 C19(H19), C21(H21)
3.d X=CH2 refined with riding coordinates:
 N4(H4A,H4B), N8(H8A,H8B)
3.e Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8C,H8D,H8E), C9(H9A,H9B,H9C)
;
_shelx_res_checksum              21717
_shelx_hkl_checksum              24217
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'