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_7055500
_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         'C16 H17 Cu N4 O9 P'
_chemical_formula_sum            'C16 H17 Cu N4 O9 P'
_chemical_formula_weight         503.85
_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
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.6819(7)
_cell_length_b                   10.5814(5)
_cell_length_c                   25.5715(14)
_cell_measurement_temperature    115
_cell_volume                     4243.2(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
'SHELXS-97, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122'
_diffrn_ambient_temperature      115.0
_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 0.998
_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  0.0334
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            20472
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.508
_diffrn_reflns_theta_min         2.816
_diffrn_source                   'X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Siemens KFF Mo 2K-180'
_exptl_absorpt_coefficient_mu    1.161
_exptl_absorpt_correction_T_max  0.74
_exptl_absorpt_correction_T_min  0.60
_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    1.577
_exptl_crystal_description       prism
_exptl_crystal_F_000             2056
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: diethyl ether / DCM'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.864
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    4
_refine_ls_number_parameters     283
_refine_ls_number_reflns         4863
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0362
_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^)+(0.0368P)^2^+4.6609P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0803
_refine_ls_wR_factor_ref         0.0889
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3724
_reflns_number_total             4863
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj03572d2.cif
_cod_data_source_block           13ma2105
_cod_depositor_comments
'Adding full bibliography for 7055499--7055503.cif.'
_cod_database_code               7055500
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.845
_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. Restrained distances
 C16-C15 \\sim C16A-C15A \\sim C14-C13
 with sigma of 0.01
 O9-C15 \\sim O9-C15A \\sim O8-C13
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C15A) = Uanis(C16A) = Uanis(C15) = Uanis(C16)
4. Others
 Fixed Sof: C15(0.75) H15A(0.75) H15B(0.75) C16(0.75) H16A(0.75) H16B(0.75)
 H16C(0.75) C15A(0.25) H15C(0.25) H15D(0.25) C16A(0.25) H16D(0.25) H16E(0.25)
 H16F(0.25)
5.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C15(H15A,H15B), C15A(H15C,H15D)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10)
5.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C16A(H16D,H16E,H16F)
;
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a mylar loop oil'
_olex2_submission_special_instructions 'No special instructions were received'