Solvothermal synthesis of enneanuclear [CuLn] clusters.
Canaj, Angelos B.; Tzimopoulos, Demetrios I.; Otręba, Marta; Lis, Tadeusz; Inglis, Ross; Milios, Constantinos J.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 19880–19885; doi:10.1039/c5dt03542b

data_7037535
_publ_section_title
;
 Solvothermal synthesis of enneanuclear [CuLn] clusters.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              19880
_journal_page_last               19885
_journal_paper_doi               10.1039/c5dt03542b
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C98 H98 Cu7 Gd2 N6 O26, 2(C2 H3 N)'
_chemical_formula_sum            'C102 H104 Cu7 Gd2 N8 O26'
_chemical_formula_weight         2617.21
_chemical_name_systematic
;
 ?
;
_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_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-09-10 deposited with the CCDC.
2015-10-29 downloaded from the CCDC.
;
_cell_angle_alpha                68.40(2)
_cell_angle_beta                 69.42(2)
_cell_angle_gamma                84.05(2)
_cell_formula_units_Z            1
_cell_length_a                   11.991(3)
_cell_length_b                   14.520(4)
_cell_length_c                   16.537(4)
_cell_measurement_reflns_used    12031
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      29
_cell_measurement_theta_min      3
_cell_volume                     2505.1(12)
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2011)'
_computing_data_collection       'CrysAlis PRO (Agilent, 2011)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2011)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'KUMA KM4 diffractometer with CCD detector'
_diffrn_measurement_method       w/
_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  0.0536
_diffrn_reflns_av_unetI/netI     0.0776
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25865
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         28.561
_diffrn_reflns_theta_min         3.019
_exptl_absorpt_coefficient_mu    2.838
_exptl_absorpt_correction_T_max  0.958
_exptl_absorpt_correction_T_min  0.477
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5
Analytical numeric absorption correction using a
multifaceted crystal model based on expressions
derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.735
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             1311
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.03
_refine_diff_density_min         -1.03
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     662
_refine_ls_number_reflns         12167
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0447
_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^)+(0.0500P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0991
_refine_ls_wR_factor_ref         0.1046
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8542
_reflns_number_total             12167
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03542b2.cif
_cod_data_source_block           AT2302A
_cod_database_code               7037535
_shelx_estimated_absorpt_t_min   0.396
_shelx_estimated_absorpt_t_max   0.945
_shelxl_version_number           2013-2
_shelx_res_checksum              14569