Two new Cu(ii) and La(iii) 2D coordination polymers, synthesis and in situ structural analysis by X-ray diffraction.
Lundvall, F.; Wragg, D. S.; Dietzel, P. D. C.; Fjellvåg, H; Dalton transactions (Cambridge, England : 2003) 45 (2016) 12827–12834; doi:10.1039/c6dt02195f

data_7040044
_publ_section_title
;
 Two new Cu(ii) and La(iii) 2D coordination polymers, synthesis and in
 situ structural analysis by X-ray diffraction.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12827
_journal_page_last               12834
_journal_paper_doi               10.1039/c6dt02195f
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         '4(H2 O), C3 H7 N O, C51 H49 La2 N O22'
_chemical_formula_sum            'C54 H64 La2 N2 O27'
_chemical_formula_weight         1450.89
_chemical_name_systematic        CPO-72-La
_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   mixed
_audit_creation_date             2016-06-23
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-07-01 deposited with the CCDC.
2016-07-25 downloaded from the CCDC.
;
_cell_angle_alpha                90.4630(10)
_cell_angle_beta                 105.8700(10)
_cell_angle_gamma                99.8160(10)
_cell_formula_units_Z            2
_cell_length_a                   13.4844(5)
_cell_length_b                   14.1740(6)
_cell_length_c                   15.6448(6)
_cell_measurement_reflns_used    9842
_cell_measurement_temperature    105(2)
_cell_measurement_theta_max      28.34
_cell_measurement_theta_min      2.43
_cell_volume                     2829.36(19)
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2007)'
_computing_data_collection       'Bruker APEX2 (Bruker, 2007)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2007)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      105.06
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker PHOTON CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_unetI/netI     0.0266
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            90197
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.349
_diffrn_reflns_theta_min         2.169
_exptl_absorpt_coefficient_mu    1.582
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5910
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.703
_exptl_crystal_description       needle
_exptl_crystal_F_000             1464
_exptl_crystal_recrystallization_method 'Solvothermal synthesis'
_exptl_crystal_size_max          0.753
_exptl_crystal_size_mid          0.302
_exptl_crystal_size_min          0.222
_refine_diff_density_max         2.989
_refine_diff_density_min         -1.316
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     837
_refine_ls_number_reflns         14080
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0316
_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^)+(0.0268P)^2^+5.2737P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0683
_refine_ls_wR_factor_ref         0.0720
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11880
_reflns_number_total             14080
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02195f2.cif
_cod_data_source_block           cpo-72-la
_cod_depositor_comments
'Adding full bibliography for 7040043--7040044.cif.'
_cod_database_code               7040044
_shelx_estimated_absorpt_t_max   0.720
_shelx_estimated_absorpt_t_min   0.382
_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, All O(H,H) groups
2. Restrained distances
 O3C-H3CD = O3C-H3CE
 0.87 with sigma of 0.02
 O4W-H4WA = O4W-H4WB
 0.87 with sigma of 0.02
 H3CD-H3CE
 1.38 with sigma of 0.04
 H4WA-H4WB
 1.38 with sigma of 0.04
 N1S-C3S \\sim N1S-C2S \\sim N2S-C5S \\sim N2S-C6S
 with sigma of 0.02
 La1-H3CD \\sim La1-H3CE
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C4S, N2S, C5S, C6S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1S, C1S, N1S, C3S, C2S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: C1S(0.75) H1S(0.75) C2S(0.75) H2SA(0.75) H2SB(0.75) H2SC(0.75)
 C3S(0.75) H3SA(0.75) H3SB(0.75) H3SC(0.75) N1S(0.75) C4S(0.25) H4S(0.25)
 C6S(0.25) H6SA(0.25) H6SB(0.25) H6SC(0.25) N2S(0.25) C5S(0.25) H5SA(0.25)
 H5SB(0.25) H5SC(0.25)
5.a Free rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB)
5.b Rotating group:
 O2C(H2CD,H2CE), O4C(H4CA,H4CB)
5.c Aromatic/amide H refined with riding coordinates:
 C1S(H1S), C1C(H1C), C2(H2), C5(H5), C6(H6), C10(H10), C13(H13), C14(H14),
 C18(H18), C21(H21), C22(H22), C26(H26), C29(H29), C30(H30), C34(H34), C37(H37),
  C38(H38), C42(H42), C45(H45), C46(H46), C4S(H4S)
5.d Idealised Me refined as rotating group:
 C2S(H2SA,H2SB,H2SC), C3S(H3SA,H3SB,H3SC), C2C(H2CA,H2CB,H2CC), C3C(H3CA,H3CB,
 H3CC), C8(H8A,H8B,H8C), C16(H16A,H16B,H16C), C24(H24A,H24B,H24C), C32(H32A,
 H32B,H32C), C40(H40A,H40B,H40C), C48(H48A,H48B,H48C), C6S(H6SA,H6SB,H6SC),
 C5S(H5SA,H5SB,H5SC)
;
_shelx_res_checksum              81683
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'