Copper(ii) complexes with phosphorylated 1,10-phenanthrolines: from molecules to infinite supramolecular arrays
Mitrofanov, Alexander Yu.; Rousselin, Yoann; Guilard, Roger; Brandès, Stéphane; Bessmertnykh-Lemeune, Alla G.; Uvarova, Marina A.; Nefedov, Sergey E.; New J. Chem. 40 (2016) 5896–; doi:10.1039/C5NJ03572D

data_7055502
_publ_section_title
;
 Copper(ii) complexes with phosphorylated 1,10-phenanthrolines: from
 molecules to infinite supramolecular arrays
;
_journal_issue                   7
_journal_name_full               'New J. Chem.'
_journal_page_first              5896
_journal_paper_doi               10.1039/C5NJ03572D
_journal_volume                  40
_journal_year                    2016
_chemical_formula_moiety         'C40 H52 Cu2 N8 O24 P4'
_chemical_formula_sum            'C40 H52 Cu2 N8 O24 P4'
_chemical_formula_weight         1279.85
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-06-24
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.23 svn.r2948 for OlexSys, GUI svn.r4855)
;
_audit_update_record
;
2014-06-24 deposited with the CCDC.
2016-04-26 downloaded from the CCDC.
;
_cell_angle_alpha                77.046(6)
_cell_angle_beta                 88.932(6)
_cell_angle_gamma                77.832(6)
_cell_formula_units_Z            1
_cell_length_a                   9.6399(12)
_cell_length_b                   12.1111(14)
_cell_length_c                   12.1162(16)
_cell_measurement_temperature    115
_cell_volume                     1347.0(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2013)'
_diffrn_ambient_temperature      115
_diffrn_detector                 'CCD Plate'
_diffrn_detector_area_resol_mean '512 x 512'
_diffrn_detector_type            APEX2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Nonius Kappa Apex II'
_diffrn_measurement_method       '\f and \w scans''
_diffrn_radiation_collimation    '0.6 mm'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0527
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            34624
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.657
_diffrn_reflns_theta_min         2.726
_diffrn_source                   'X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Siemens KFF Mo 2K-180'
_exptl_absorpt_coefficient_mu    0.997
_exptl_absorpt_correction_T_max  0.74
_exptl_absorpt_correction_T_min  0.62
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'clear light blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_description       prism
_exptl_crystal_F_000             658
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: diethyl ether / DCM'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.564
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     356
_refine_ls_number_reflns         6260
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0336
_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^)+(0.0351P)^2^+0.8394P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0756
_refine_ls_wR_factor_ref         0.0813
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5073
_reflns_number_total             6260
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj03572d2.cif
_cod_data_source_block           13al2406
_cod_depositor_comments
'Adding full bibliography for 7055499--7055503.cif.'
_cod_database_code               7055502
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.789
_shelx_estimated_absorpt_t_min   0.722
_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.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C15(H15A,H15B), C13(H13A,H13B), C19(H19A,H19B)
2.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C8(H8), C7(H7), C1(H1), C12(H12), C2(H2)
2.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C14(H14A,H14B,
 H14C)
;
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a mylar loop oil'
_olex2_submission_special_instructions 'No special instructions were received'