Brightly phosphorescent tetranuclear copper(i) pyrazolates.
Dias, H. V. Rasika; Diyabalanage, Himashinie V. K.; Ghimire, Mukunda M.; Hudson, Joshua M.; Parasar, Devaborniny; Palehepitiya Gamage, Chammi S.; Li, Shan; Omary, Mohammad A.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 14979–14983; doi:10.1039/c9dt03402a

data_7701252
_publ_section_title
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 Brightly phosphorescent tetranuclear copper(i) pyrazolates.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14979
_journal_page_last               14983
_journal_paper_doi               10.1039/c9dt03402a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C36 H56 Br4 Cu4 N8'
_chemical_formula_sum            'C36 H56 Br4 Cu4 N8'
_chemical_formula_weight         1174.68
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_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
_audit_creation_date             2016-12-05
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_audit_update_record
;
2019-06-27 deposited with the CCDC.    2019-09-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.9169(15)
_cell_length_b                   20.9151(16)
_cell_length_c                   22.8836(17)
_cell_measurement_reflns_used    9188
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.05
_cell_measurement_theta_min      2.36
_cell_volume                     9053.9(12)
_computing_cell_refinement       'SAINT V7.16B (?, 2016)'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'SAINT V7.16B (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0655
_diffrn_reflns_av_unetI/netI     0.0397
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            68234
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.996
_diffrn_reflns_theta_min         1.947
_exptl_absorpt_coefficient_mu    5.419
_exptl_absorpt_correction_T_max  0.7887
_exptl_absorpt_correction_T_min  0.569455
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.1166 before and 0.0389 after correction.
The Ratio of minimum to maximum transmission is 0.5695.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.724
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelpipe
_exptl_crystal_F_000             4672
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.046
_refine_diff_density_max         1.019
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         8902
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0344
_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^)+(0.0357P)^2^+10.4465P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0711
_refine_ls_wR_factor_ref         0.0828
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6438
_reflns_number_total             8902
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03402a2.cif
_cod_data_source_block           dias343s
_cod_depositor_comments
'Adding full bibliography for 7701251--7701253.cif.'
_cod_database_code               7701252
_shelx_estimated_absorpt_t_max   0.789
_shelx_estimated_absorpt_t_min   0.369
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C16A-C17A = C16A-C18A = C16B-C17B = C16B-C18B
 1.53 with sigma of 0.02
 C12-C16A = C12-C16B
 1.5 with sigma of 0.01
 C16A-C18A \\sim C16B-C18B
 with sigma of 0.02
 C16A-C17A \\sim C16B-C17B
 with sigma of 0.02
 C12-C16A \\sim C12-C16B
 with sigma of 0.02
 C34-C30 \\sim C34A-C30
 with sigma of 0.008
 C35-C34 \\sim C35A-C34A \\sim C36A-C34A \\sim C36-C34
 with sigma of 0.008
3. Uiso/Uaniso restraints and constraints
Uanis(C16B) \\sim Ueq: with sigma of 0.008 and sigma for terminal atoms of 0.008
Uanis(C35) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C36) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.005
Uanis(C18B) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(C18A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
4. Others
 Sof(C16B)=Sof(H16B)=Sof(C17B)=Sof(H17D)=Sof(H17E)=Sof(H17F)=Sof(C18B)=
 Sof(H18D)=Sof(H18E)=Sof(H18F)=1-FVAR(1)
 Sof(C16A)=Sof(H16A)=Sof(C17A)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C18A)=
 Sof(H18A)=Sof(H18B)=Sof(H18C)=FVAR(1)
 Sof(C34A)=Sof(H34A)=Sof(C35A)=Sof(H35D)=Sof(H35E)=Sof(H35F)=Sof(C36A)=
 Sof(H36D)=Sof(H36E)=Sof(H36F)=1-FVAR(2)
 Sof(C34)=Sof(H34)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=Sof(C36)=Sof(H36A)=
 Sof(H36B)=Sof(H36C)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C4(H4), C7(H7), C13(H13), C16A(H16A), C16B(H16B), C22(H22), C25(H25),
 C31(H31), C34(H34), C34A(H34A)
5.b Me refined with riding coordinates:
 C17A(H17A,H17B,H17C), C18A(H18A,H18B,H18C), C17B(H17D,H17E,H17F), C18B(H18D,
 H18E,H18F)
5.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C14(H14A,
 H14B,H14C), C15(H15A,H15B,H15C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C),
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C32(H32A,H32B,H32C), C33(H33A,H33B,
 H33C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C35A(H35D,H35E,H35F),
 C36A(H36D,H36E,H36F)
;
_shelx_res_checksum              75269
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'