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_7055503
_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         'C20 H26 Cu N4 O12 P2'
_chemical_formula_sum            'C20 H26 Cu N4 O12 P2'
_chemical_formula_weight         639.93
_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             2015-02-03
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-02-16 deposited with the CCDC.
2016-04-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.2508(6)
_cell_length_b                   9.2040(4)
_cell_length_c                   34.9028(15)
_cell_measurement_reflns_used    9867
_cell_measurement_temperature    100
_cell_measurement_theta_max      68.377
_cell_measurement_theta_min      3.716
_cell_volume                     5220.5(4)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 CMOS
_diffrn_detector_area_resol_mean '1024 x 1024'
_diffrn_detector_type            'Photon 100'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans''
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'QUAZAR MX multilayer optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            26677
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.463
_diffrn_reflns_theta_min         3.716
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Cu
_diffrn_source_type              'high brilliance microfocus sealed tube, Cu'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.971
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.6418
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0828 before and 0.0595 after correction.
The Ratio of minimum to maximum transmission is 0.8522.
The \l/2 correction factor is 0.00150.
;
_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    1.628
_exptl_crystal_description       prism
_exptl_crystal_F_000             2632
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: heptane'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.141
_refine_diff_density_min         -1.458
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.181
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    22
_refine_ls_number_parameters     331
_refine_ls_number_reflns         4744
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.186
_refine_ls_R_factor_all          0.1029
_refine_ls_R_factor_gt           0.0994
_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^)+(0.0740P)^2^+64.6063P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2459
_refine_ls_wR_factor_ref         0.2480
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4457
_reflns_number_total             4744
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj03572d2.cif
_cod_data_source_block           cu_15ami230_0ma
_cod_depositor_comments
'Adding full bibliography for 7055499--7055503.cif.'
_cod_database_code               7055503
_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
2. Restrained distances
 O5-C17A \\sim O5-C19 \\sim O6-C17 \\sim O6-C19A \\sim O1-C1 \\sim O1A-C1 \\sim
O3A-C3A \\sim O3-C3
 with sigma of 0.02
 C2-C1 \\sim C4A-C3A \\sim C4-C3 \\sim C20-C19 \\sim C18A-C17A \\sim C20A-C19A
\\sim C18-C17
 with sigma of 0.02
 P2-O4 \\sim P1A-O2A \\sim P1-O2
 with sigma of 0.02
 P1-O1 \\sim P1A-O1A \\sim P1A-O3A \\sim P1-O3 \\sim P2-O5 \\sim P2-O6
 with sigma of 0.02
 P1A-C5 \\sim P1-C5 \\sim P2-C12
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C3) = Uanis(C3A) = Uanis(C4) = Uanis(C4A) = Uanis(O3A) = Uanis(O3) =
Uanis(O2) = Uanis(O2A) = Uanis(P1) = Uanis(O1A) = Uanis(O1) = Uanis(C1) =
Uanis(C2) = Uanis(P1A)
Uanis(C17A) = Uanis(C19) = Uanis(C20) = Uanis(C18A) = Uanis(C19A) = Uanis(C17)
= Uanis(C18) = Uanis(C20A)
4. Others
 Sof(C17A)=Sof(H17C)=Sof(H17D)=Sof(C18A)=Sof(H18D)=Sof(H18E)=Sof(H18F)=
 Sof(C19A)=Sof(H19C)=Sof(H19D)=Sof(C20A)=Sof(H20D)=Sof(H20E)=Sof(H20F)=1-FVAR(1)
 Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(C19)=
 Sof(H19A)=Sof(H19B)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=FVAR(1)
 Sof(H1BC)=Sof(H1BD)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=
 Sof(H4AC)=Sof(O1A)=Sof(O2A)=Sof(O3A)=Sof(P1A)=1-FVAR(2)
 Sof(H1AB)=Sof(H1AA)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C4)=Sof(H4A)=Sof(H4B)=
 Sof(H4C)=Sof(O1)=Sof(O2)=Sof(O3)=Sof(P1)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1AB,H1AA), C1(H1BC,H1BD), C3(H3A,H3B), C3A(H3AA,H3AB), C17(H17A,H17B),
 C17A(H17C,H17D), C19(H19A,H19B), C19A(H19C,H19D)
5.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), C9(H9), C11(H11), C13(H13), C16(H16)
5.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C4A(H4AA,H4AB,H4AC), C18(H18A,H18B,H18C),
 C18A(H18D,H18E,H18F), C20(H20A,H20B,H20C), C20A(H20D,H20E,H20F)
;
_shelx_shelxl_version_number     2014/7
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder oil'
_olex2_submission_special_instructions 'No special instructions were received'