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_7055499
_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         'C32 H36 Cu N5 O10 P2, N O3'
_chemical_formula_sum            'C32 H36 Cu N6 O13 P2'
_chemical_formula_weight         838.15
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_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                90
_cell_angle_beta                 92.779(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.6371(6)
_cell_length_b                   7.9394(2)
_cell_length_c                   23.7780(8)
_cell_measurement_temperature    115
_cell_volume                     3514.23(19)
_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 0.999
_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  0.0815
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            152871
_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         27.603
_diffrn_reflns_theta_min         2.705
_diffrn_source                   'X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Siemens KFF Mo 2K-180'
_exptl_absorpt_coefficient_mu    0.789
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_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    1.584
_exptl_crystal_description       prism
_exptl_crystal_F_000             1732
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: diethyl ether / DCM'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.879
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    6
_refine_ls_number_parameters     490
_refine_ls_number_reflns         8162
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0421P)^2^+5.8343P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0966
_refine_ls_wR_factor_ref         0.1055
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6676
_reflns_number_total             8162
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj03572d2.cif
_cod_data_source_block           12am0511
_cod_depositor_comments
'Adding full bibliography for 7055499--7055503.cif.'
_cod_database_code               7055499
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.925
_shelx_estimated_absorpt_t_min   0.911
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Rigid bond restraints
 P2, O6A, O6B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
3. Uiso/Uaniso restraints and constraints
Uanis(O6A) = Uanis(O6B) = Uanis(C25B) = Uanis(C25A) = Uanis(C26A) = Uanis(C26B)
4. Same fragment restrains
{O6A, C25A, C26A}
as
{O6B, C25B, C26B}
5. Others
 Fixed Sof: O6A(0.83583) C25A(0.83583) H25A(0.83583) H25B(0.83583)
 C26A(0.83583) H26A(0.83583) H26B(0.83583) H26C(0.83583) C28A(0.5) H28A(0.5)
 H28B(0.5) H28C(0.5) O6B(0.16417) C25B(0.16417) H25C(0.16417) H25D(0.16417)
 C26B(0.16417) H26D(0.16417) H26E(0.16417) H26F(0.16417) C28B(0.5) H28D(0.5)
 H28E(0.5) H28F(0.5) H27A(0.5) H27B(0.5) H27C(0.5) H27D(0.5)
6.a Rotating group:
 O13(H13A,H13B)
6.b Secondary CH2 refined with riding coordinates:
 C25A(H25A,H25B), C25B(H25C,H25D), C27(H27A,H27B), C27(H27C,H27D), C29(H29A,
 H29B), C31(H31A,H31B)
6.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C10(H10), C13(H13), C14(H14),
 C15(H15), C17(H17), C18(H18), C20(H20), C22(H22)
6.d Idealised Me refined as rotating group:
 C26A(H26A,H26B,H26C), C28A(H28A,H28B,H28C), C26B(H26D,H26E,H26F), C28B(H28D,
 H28E,H28F), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C)
;
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a mylar loop oil'
_olex2_submission_special_instructions 'No special instructions were received'