Construction of copper chains with new fluorescent guanidino-functionalized naphthyridine ligands.
Krämer, Christoph; Leingang, Simone; Hübner, Olaf; Kaifer, Elisabeth; Wadepohl, Hubert; Himmel, Hans-Jörg; Dalton transactions (Cambridge, England : 2003) 45 (2016) 16966–16983; doi:10.1039/c6dt03166h

data_7040782
_publ_section_title
;
 Construction of copper chains with new fluorescent
 guanidino-functionalized naphthyridine ligands.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16966
_journal_page_last               16983
_journal_paper_doi               10.1039/c6dt03166h
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety
'C36 H56 Cl4 Cu6 N16, 2(C36 H56 Cu4 N16), 10(B F4), 8(C H2 Cl2)'
_chemical_formula_sum            'C116 H184 B10 Cl20 Cu14 F40 N48'
_chemical_formula_weight         4717.76
_chemical_properties_physical    air-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                hi_ck2
_audit_creation_date             2015-11-03
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-09-23 deposited with the CCDC.
2016-09-26 downloaded from the CCDC.
;
_cell_angle_alpha                100.103(2)
_cell_angle_beta                 100.290(2)
_cell_angle_gamma                91.496(2)
_cell_formula_units_Z            1
_cell_length_a                   12.7803(3)
_cell_length_b                   15.1583(4)
_cell_length_c                   23.8968(6)
_cell_measurement_reflns_used    29243
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      28.2930
_cell_measurement_theta_min      3.4650
_cell_volume                     4476.5(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material
'encif (Wadepohl, 2009-15); encifer 1.5 (CCDC, 2014)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_diffrn_ambient_environment      perfluoro
_diffrn_ambient_temperature      120(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  1  \w    -44.00  56.00   0.50   15.00    --   26.43 -77.00  30.00  200
  2  \w      5.00  95.00   0.50   15.00    --   26.43  57.00 150.00  180
  3  \w    -42.00  47.00   0.50   15.00    --   26.43 -57.00 -90.00  178
  4  \w     -4.00  97.00   0.50   15.00    --   26.43  77.00  30.00  202
  5  \f     81.00 119.00   0.50   15.00  26.43  26.43 -40.00    --    76
  6  \w    -20.00  68.00   0.50   15.00    --   26.43 -99.00   0.00  176
  7  \w     -4.00  97.00   0.50   15.00    --   26.43  77.00 -60.00  202
  8  \w     -4.00  97.00   0.50   15.00    --   26.43  77.00-180.00  202
  9  \w    -46.00  52.00   0.50   15.00    --   26.43 -38.00-180.00  196
 10  \w     -4.00  97.00   0.50   15.00    --   26.43  77.00  60.00  202
 11  \w      1.00  99.00   0.50   15.00    --   26.43  38.00 -90.00  196
 12  \w     -6.00  78.00   0.50   15.00    --   26.43-116.00 166.00  168
 13  \w    -42.00  47.00   0.50   15.00    --   26.43 -57.00  90.00  178
 14  \w    -20.00  68.00   0.50   15.00    --   26.43 -99.00 -90.00  176
 15  \w    -42.00  47.00   0.50   15.00    --   26.43 -57.00-150.00  178
 16  \w      5.00  92.00   0.50   15.00    --   26.43  57.00 -90.00  174
 17  \w      7.00  70.00   0.50   15.00    --   26.43  38.00  60.00  126
 18  \w     -4.00  97.00   0.50   25.00    --   26.43  77.00-150.00  202
 19  \w     -4.00  97.00   0.50   25.00    --   26.43  77.00-120.00  202
 20  \w     -4.00  97.00   0.50   25.00    --   26.43  77.00 -90.00  202
 21  \w     -4.00  97.00   0.50   25.00    --   26.43  77.00 -60.00  202
 22  \w     -4.00  65.00   0.50   25.00    --   26.43  77.00 -30.00  138
 23  \w     -4.00  35.00   0.50   25.00    --   26.43  77.00-180.00   78
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0254079000
_diffrn_orient_matrix_UB_12      0.0283166000
_diffrn_orient_matrix_UB_13      0.0260134000
_diffrn_orient_matrix_UB_21      -0.0334961000
_diffrn_orient_matrix_UB_22      -0.0200420000
_diffrn_orient_matrix_UB_23      0.0155423000
_diffrn_orient_matrix_UB_31      0.0377545000
_diffrn_orient_matrix_UB_32      -0.0326121000
_diffrn_orient_matrix_UB_33      0.0048329000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0833
_diffrn_reflns_av_unetI/netI     0.0436
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            165973
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.246
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.024
_exptl_absorpt_correction_T_max  0.912
_exptl_absorpt_correction_T_min  0.865
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
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_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.750
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2372
_exptl_crystal_size_max          0.101
_exptl_crystal_size_mid          0.079
_exptl_crystal_size_min          0.062
_refine_diff_density_max         2.650
_refine_diff_density_min         -1.236
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1141
_refine_ls_number_reflns         18252
_refine_ls_number_restraints     485
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0486
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0465P)^2^+14.1373P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1096
_refine_ls_wR_factor_ref         0.1191
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14220
_reflns_number_total             18252
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt03166h2.cif
_cod_data_source_block           hi_ck2
_cod_depositor_comments
'Adding full bibliography for 7040782--7040791.cif.'
_cod_database_code               7040782
_audit_block_refno               2561
_audit_block_usercomment         'ckrh04 irregular yellow'
_chemical_oxdiff_formula         'C116 H184 B10 Cl20 Cu14 F40 N48'
_chemical_oxdiff_usercomment     'ckrh04 irregular yellow'
_shelx_estimated_absorpt_t_max   0.823
_shelx_estimated_absorpt_t_min   0.823
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_shelxl_version_number           2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 B1-F11 \\sim B1-F12 \\sim B1-F13 \\sim B1-F14
 with sigma of 0.02
 F11-F12 \\sim F11-F13 \\sim F11-F14 \\sim F12-F13 \\sim F12-F14 \\sim F13-F14
 with sigma of 0.02
 C61-Cl61 \\sim C61-Cl62
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C61, C71, C81, C91, Cl41, Cl42, Cl61, Cl62, Cl71, Cl72, Cl81, Cl82, Cl91, Cl92
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 B1, B2, B3, B4, B5, F11, F12, F13, F14, F21, F22, F23, F24, F31, F32, F33,
 F34, F41, F42, F43, F44, F51, F52, F53, F54
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Same fragment restrains
{F11, F12, F13, F14, B1} sigma for 1-2: 0.02, 1-3: 0.04
as
{F21, F22, F23, F24, B2}
{F11, F12, F13, F14, B1} sigma for 1-2: 0.02, 1-3: 0.04
as
{F31, F32, F33, F34, B3}
{F11, F12, F13, F14, B1} sigma for 1-2: 0.02, 1-3: 0.04
as
{F41, F42, F43, F44, B4}
{F11, F12, F13, F14, B1} sigma for 1-2: 0.02, 1-3: 0.04
as
{F51, F52, F53, F54, B5}
{Cl61, Cl62, C61} sigma for 1-2: 0.02, 1-3: 0.04
as
{Cl71, Cl72, C71}
{Cl61, Cl62, C61} sigma for 1-2: 0.02, 1-3: 0.04
as
{Cl81, Cl82, C81}
{Cl61, Cl62, C61} sigma for 1-2: 0.02, 1-3: 0.04
as
{Cl91, Cl92, C91}
5.a Secondary CH2 refined with riding coordinates:
 C61(H61A,H61B), C71(H71A,H71B), C81(H81A,H81B), C91(H91A,H91B)
5.b Aromatic/amide H refined with riding coordinates:
 C42(H42), C43(H43), C45(H45), C46(H46), C22(H22), C23(H23), C25(H25),
 C26(H26), C2(H2), C3(H3), C5(H5), C6(H6)
5.c Idealised Me refined as rotating group:
 C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C53(H53A,H53B,
 H53C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C58(H58A,
 H58B,H58C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C),
 C33(H33A,H33B,H33C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,
 H37C), C38(H38A,H38B,H38C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,
 H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C),
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              19879
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.133
_oxdiff_exptl_absorpt_empirical_full_min 0.920
_cell_oxdiff_length_a            12.7803(3)
_cell_oxdiff_length_b            15.1583(4)
_cell_oxdiff_length_c            23.8968(6)
_cell_oxdiff_angle_alpha         100.103(2)
_cell_oxdiff_angle_beta          100.290(2)
_cell_oxdiff_angle_gamma         91.496(2)
_cell_oxdiff_volume              4476.5(2)
_cell_oxdiff_measurement_reflns_used 29243