Subtle Modulation of Cu4X4L2 Phosphine Cluster Cores Leads to Changes in Luminescence.
Chen, Kelly; Shearer, Jason; Catalano, Vincent J.; Inorganic chemistry 54 (2015) 6245–6256; doi:10.1021/acs.inorgchem.5b00443

data_4343306
_publ_section_title
;
 Subtle Modulation of Cu4X4L2 Phosphine Cluster Cores Leads to Changes in
 Luminescence.
;
_journal_issue                   13
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6245
_journal_page_last               6256
_journal_paper_doi               10.1021/acs.inorgchem.5b00443
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C19 H12 Cl2 Cu2 N2 P, 0.5(O)'
_chemical_formula_sum            'C19 H12 Cl2 Cu2 N2 O0.5 P'
_chemical_formula_weight         505.26
_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   geom
_audit_creation_date             2014-01-29
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_cell_angle_alpha                103.5980(10)
_cell_angle_beta                 93.2370(10)
_cell_angle_gamma                95.7600(10)
_cell_formula_units_Z            2
_cell_length_a                   9.3487(7)
_cell_length_b                   10.0979(7)
_cell_length_c                   11.1299(8)
_cell_measurement_reflns_used    5327
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.373
_cell_measurement_theta_min      2.197
_cell_volume                     1012.59(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            18217
_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         25.492
_diffrn_reflns_theta_min         1.889
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.451
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6760
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0679 before and 0.0520 after correction. The Ratio of minimum to maximum transmission is 0.9060. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            clear
_exptl_crystal_colour_lustre     clear
_exptl_crystal_density_diffrn    1.657
_exptl_crystal_description       block
_exptl_crystal_F_000             502
_exptl_crystal_size_max          0.146
_exptl_crystal_size_mid          0.141
_exptl_crystal_size_min          0.129
_refine_diff_density_max         0.759
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         3757
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0292
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0374P)^2^+1.3089P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0726
_refine_ls_wR_factor_ref         0.0753
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3276
_reflns_number_total             3757
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00443_si_002.cif
_cod_data_source_block           kc138_0m
_cod_depositor_comments
'Adding full bibliography for 4343305--4343312.cif.'
_cod_original_formula_sum        'C19 H12 Cl2 Cu2 N2 O0.50 P'
_cod_database_code               4343306
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.743
_shelx_estimated_absorpt_t_min   0.716
_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. Others
 Sof(C12A)=Sof(C11A)=Sof(C10A)=Sof(C9A)=Sof(C8A)=1-FVAR(1)
 Sof(C12)=Sof(C11)=Sof(C10)=Sof(C9)=Sof(C8)=FVAR(1)
 Fixed Sof: O1S(0.25) O2S(0.25)
3.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C16(H16), C17(H17), C6(H6), C5(H5), C4(H4), C3(H3), C2(H2)
3.b Idealised Me refined as rotating group:
 C19(H19a,H19b,H19c)
;